CN106366444A - Graphene fluoride modified resin plate and preparation method thereof - Google Patents
Graphene fluoride modified resin plate and preparation method thereof Download PDFInfo
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- CN106366444A CN106366444A CN201610805726.1A CN201610805726A CN106366444A CN 106366444 A CN106366444 A CN 106366444A CN 201610805726 A CN201610805726 A CN 201610805726A CN 106366444 A CN106366444 A CN 106366444A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08L61/24—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with urea or thiourea
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a preparation method of a graphene fluoride modified resin plate. The preparation method comprises the following steps of: mixing graphene fluoride, resin, hydroxypropyl methyl cellulose, glycol ether, texanol, dibutyl phthalate, dimethyl siloxane and water, then carrying out heat treatment, and finally carrying out compression molding to prepare the graphene fluoride modified resin plate, wherein relative to 100 parts of resin in parts by weight, the using amount of graphene fluoride is 6 to 10 parts by weight, the using amount of hydroxypropyl methyl cellulose is 1 to 9 parts by weight, the using amount of glycol ether is 1 to 5 parts by weight, the using amount of texanol is 1 to 5 parts by weight, the using amount of dibutyl phthalate is 1 to 3 parts by weight, the using amount of dimethyl siloxane is 1 to 3 parts by weight, and the using amount of water is 80 to 150 parts by weight. The graphene fluoride modified resin plate has extremely good insulativity and high mechanical strength and tenacity.
Description
Technical field
The present invention relates to resin plate is and in particular to fluorinated graphene modified resin plate and preparation method thereof.
Background technology
Resin plate is to be mixed after Overheating Treatment by one or more high molecular polymers, and the tabular that compression molding obtains is produced
Product, resin plate has the excellent performance such as excellent resistance to acids and bases and resistance to leakage property, and therefore resin plate is of many uses.Resin
Plate is often used as the case material of insulating device, and the shell of some household electrical appliance or automotive trim product.Therefore, resin plate
Insulating properties and mechanical strength are very important performance indications.
Content of the invention
It is an object of the invention to provide a kind of fluorinated graphene modified resin plate, this fluorinated graphene modified resin plate has
Insulating properties and high mechanical strength and toughness well.
To achieve these goals, the invention provides a kind of preparation method of fluorinated graphene modified resin plate, comprising:
By fluorinated graphene, resin, hydroxypropyl methyl cellulose, ethylene glycol, alcohol ester 12 (as 2,2,4- trimethyl -1,3-
Pentanediol mono isobutyrate), dibutyl phthalate, dimethyl siloxane and water mixing, then carry out heat treatment, rear mold
Molded prepared fluorinated graphene modified resin plate；
Wherein, with respect to the resin of 100 weight portions, the consumption of fluorinated graphene is 6-10 weight portion, and hydroxypropyl methyl is fine
The consumption of dimension element is 1-9 weight portion, and the consumption of ethylene glycol is 1-5 weight portion, and the consumption of alcohol ester 12 is 1-5 weight portion,
The consumption of dibutyl phthalate measures part for 1-3, and the consumption of dimethyl siloxane measures part for 1-3, and the consumption of water is 80-150
Weight portion.
The preparation of fluorinated graphene is further comprises in the preparation method of fluorinated graphene modified resin plate that the present invention provides
Method: hf solution is added in graphene oxide solution carry out ultrasonic, be mixed to get mixed liquor；Again described mixed liquor is proceeded to
Heated in an oven in reactor；After natural cooling, drying just obtains fluorinated graphene.
During preparing fluorinated graphene, in order to improve the incorporation of fluorine and then improve insulation and the machine of resin plate
It is preferable that the concentration of graphene oxide solution is 5-10mg/ml, the mass fraction of described hf solution is 30-40% to tool intensity.
In order to improve the preparation rate of fluorinated graphene it is preferable that the power of ultrasonic generator is 40-90w, described ultrasonic
Time is 1-3min；Preferably, the temperature of heating is 180-190 DEG C, and the time is 20-24h.
In order to improve the mechanical strength of resin plate it is preferable that resin is selected from acrylic resin, polyvinyl resin, phenolic aldehyde tree
One or more of fat or polyurethane resin.Preferably, the weight average molecular weight of acrylic resin is 10,000-2 ten thousand, polyethylene tree
The weight average molecular weight of fat is 20,000-4 ten thousand, and the weight average molecular weight of phenolic resin is 10,000-2 ten thousand, the weight average molecular weight of polyurethane resin
For 10,000-2 ten thousand.
In the preparation process of resin plate, heat treatment is carried out to the raw material of mixing, in order to improve the molding effect of resin plate,
Preferably, the temperature of heat treatment is 180-200 DEG C, and the time of heat treatment is 0.5-1.5h.
Preferably, compression molding temperature be 170-175 DEG C
Present invention also offers a kind of fluorinated graphene modified resin plate being obtained by above-mentioned preparation method.
By technique scheme, the present invention passes through to add fluorinated graphene to improve the machinery of resin plate in resin raw material
Intensity and insulating properties.With the addition of again hydroxypropyl methyl cellulose, ethylene glycol, alcohol ester 12, dibutyl phthalate,
The auxiliary agents such as dimethyl siloxane, by each raw material between strengthening synergism obtain the fluorinated graphene modified resin of high intensity
Plate.In the present invention, the preparing raw material of fluorinated graphene is graphene oxide, and graphene oxide can reach more than 100 DEG C in temperature
Hydrothermal treatment consists in be directly reduced into Graphene, the introducing of a large amount of f simultaneously greatly reduce Graphene electric conductivity thus
The mechanical strength of Graphene and pliability can be made full use of to improve mechanical strength and the toughness of resin plate.And hydroxypropyl methyl
Cellulose must add the mechanical strength also improving resin plate and molding effect.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that it is described herein concrete
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
Hereinafter will be described the present invention by embodiment.
Preparation example 1
The preparation of fluorinated graphene: the hf solution that 1ml mass fraction is 40% is added to the graphite oxide solution of 100ml
In (concentration is 10mg/ml), carries out ultrasonic 2minm in power selection 60w of ultrasonic generation, be then transferred to temperature in reactor
Select 190 DEG C to carry out heating 20h, after natural cooling, obtain fluorinated graphene.
Preparation example 2
The preparation of fluorinated graphene: the hf solution that 2ml mass fraction is 35% is added to the graphite oxide solution of 100ml
In, carry out ultrasonic 3minm in power selection 50w of ultrasonic generation, be then transferred to temperature in reactor and select 180 DEG C to carry out adding
Hot 24h, obtains fluorinated graphene after natural cooling.
Embodiment 1
By fluorinated graphene, acrylic resin (weight average molecular weight is 10,000), phenolic resin (weight average molecular weight is 20,000), hydroxyl
Propyl methocel, ethylene glycol, alcohol ester 12, dibutyl phthalate, dimethyl siloxane and water are according to weight
Proportioning is mixed for 6:50:50:2:1:1:1:1:85；Then carry out heat treatment 1.5h at 180 DEG C；Finally at 175 DEG C
Compression molding is obtained fluorinated graphene modified resin plate, is denoted as a1.
Wherein, fluorinated graphene used is to be prepared by preparation example 1.
Embodiment 2
By fluorinated graphene, polyvinyl resin (weight average molecular weight be 40,000), hydroxypropyl methyl cellulose, ethylene glycol,
Alcohol ester 12, dibutyl phthalate, dimethyl siloxane and water enter for 8:100:6:3:3:2:2:125 according to weight proportion
Row mixing；Then carry out heat treatment 1.0h at 190 DEG C；The last modified tree of the prepared fluorinated graphene of compression molding at 170 DEG C
Fat plate, is denoted as a2.
Wherein, fluorinated graphene used is to be prepared by preparation example 2.
Embodiment 3
By fluorinated graphene, polyurethane resin (weight average molecular weight be 20,000), hydroxypropyl methyl cellulose, ethylene glycol,
Alcohol ester 12, dibutyl phthalate, dimethyl siloxane and water are 10:100:9:5:5:3:3:150 according to weight proportion
Mixed；Then carry out heat treatment 0.5h at 200 DEG C；Last compression molding prepared fluorinated graphene modification at 175 DEG C
Resin plate, is denoted as a3.
Wherein, fluorinated graphene used is to be prepared by preparation example 2
Comparative example 1
Method according to embodiment 1 is obtained resin plate b1, except that not adding fluorinated graphene.
Comparative example 2
Method according to embodiment 2 is obtained resin plate b2, except that not adding fluorinated graphene.
Comparative example 3
Method according to embodiment 3 is obtained resin plate b3, except that not adding fluorinated graphene.
Comparative example 4
Method according to embodiment 1 is obtained resin plate b4, except that not adding hydroxypropyl methyl cellulose.
Comparative example 4
Method according to embodiment 1 is obtained resin plate b5, except that not adding alcohol ester 12.
Detection example 1
Fluorinated graphene modified resin plate a1-a3 and resin plate b1-b5 are first processed at 165 DEG C 2h, then then at-
Process 2h at 15 DEG C, finally carry out tensile strength (rm/mpa) and shrinkage factor (δ/%) according to the method for GB gb/t13022-91
Parameter testing, concrete outcome is shown in Table 1.
Table 1
| rm/mpa | δ/% | |
| a1 | 61.2 | 2.1 |
| a2 | 62.3 | 2.3 |
| a3 | 64.9 | 2.0 |
| b1 | 50.6 | 4.3 |
| b2 | 51.1 | 4.2 |
| b3 | 52.4 | 4.7 |
| b4 | 58.3 | 4.1 |
| b5 | 56.8 | 3.5 |
Detect 25-30 DEG C according to the method for GB gb/t13022-91, the fluorinated graphene modified resin plate under 1atm resists
Tensile strength scope is 63-70mpa.By detect example 1 it was found that the present invention provide fluorinated graphene modified resin plate exist
165 DEG C and in -15 DEG C process after tensile strength all between 60-66mpa；I.e. significantly reducing does not occur in tensile strength.
In addition, carrying out leakage testses, result shows that the fluorinated graphene modified resin plate that the present invention provides maintains very well
Insulating properties；Additionally, with the addition of hydroxypropyl methyl cellulose in the preparation process of resin plate again to significantly increase resin plate
Thermoplasticity, improves the molding effect of fluorinated graphene modified resin plate.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, multiple simple variant can be carried out to technical scheme, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy no longer separately illustrates.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it equally should be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of fluorinated graphene modified resin plate is it is characterised in that include: by fluorinated graphene, resin, hydroxyl
Propyl methocel, ethylene glycol, alcohol ester 12, dibutyl phthalate, dimethyl siloxane and water mixing, then
Carry out heat treatment, last compression molding is obtained fluorinated graphene modified resin plate；
Wherein, with respect to the resin of 100 weight portions, the consumption of described fluorinated graphene is 6-10 weight portion, described hydroxypropyl first
The consumption of base cellulose is 1-9 weight portion, and the consumption of described ethylene glycol is 1-5 weight portion, the consumption of described alcohol ester 12
For 1-5 weight portion, the consumption of described dibutyl phthalate measures part for 1-3, and the consumption of described dimethyl siloxane is 1-3 amount
Part, the consumption of described water is 80-150 weight portion.
2. preparation method according to claim 1, wherein, described preparation method also includes: hf solution is added to oxidation
Carry out in graphene solution ultrasonic, be mixed to get mixed liquor；Again described mixed liquor is transferred in reactor and carries out in an oven
Heating；After natural cooling, drying just obtains fluorinated graphene.
3. preparation method according to claim 1, wherein, the concentration of described graphene oxide solution is 5-10mg/ml, institute
The mass fraction stating hf solution is 30-40%.
4. the preparation method according to any one in claim 1-3, wherein, the power of described ultrasonic generator is 40-
70w, the described ultrasonic time is 1-3min.
5. preparation method according to claim 4, wherein, the temperature of described heating is 180-190 DEG C, and the time is 20-
24h.
6. preparation method according to claim 5, wherein, described resin is selected from acrylic resin, polyvinyl resin, phenol
One or more of urea formaldehyde or polyurethane resin.
7. preparation method according to claim 6, wherein, the weight average molecular weight of described acrylic resin is 10,000-2 ten thousand, gathers
The weight average molecular weight of vinyl is 20,000 polyvinyl resins, and the weight average molecular weight of phenolic resin is 20,000-4 ten thousand, polyurethane resin
Weight average molecular weight be 10,000-2 ten thousand.
8. preparation method according to claim 7, wherein, the temperature of described heat treatment is 180-200 DEG C, heat treatment when
Between be 0.5-1.5h.
9. preparation method according to claim 1, wherein, described compression molding temperature be 170-175 DEG C.
10. a kind of fluorinated graphene modified resin plate is it is characterised in that described fluorinated graphene modified resin plate is by claim
Preparation method described in any one in 1-9 is prepared.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610805726.1A CN106366444A (en) | 2016-09-07 | 2016-09-07 | Graphene fluoride modified resin plate and preparation method thereof |
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| CN201610805726.1A CN106366444A (en) | 2016-09-07 | 2016-09-07 | Graphene fluoride modified resin plate and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587047A (en) * | 2018-03-22 | 2018-09-28 | 长沙小新新能源科技有限公司 | A kind of fluorinated plastic and preparation method thereof |
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| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
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| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
| CN103772981A (en) * | 2013-12-30 | 2014-05-07 | 四川大学 | Low-dielectric-constant polymer/fluorinated graphene composite material and preparation method thereof |
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| CN108587047A (en) * | 2018-03-22 | 2018-09-28 | 长沙小新新能源科技有限公司 | A kind of fluorinated plastic and preparation method thereof |
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Application publication date: 20170201 |