CN108084306A - A kind of preparation method of modified graphene and its application for preparing EPS - Google Patents
A kind of preparation method of modified graphene and its application for preparing EPS Download PDFInfo
- Publication number
- CN108084306A CN108084306A CN201711225261.3A CN201711225261A CN108084306A CN 108084306 A CN108084306 A CN 108084306A CN 201711225261 A CN201711225261 A CN 201711225261A CN 108084306 A CN108084306 A CN 108084306A
- Authority
- CN
- China
- Prior art keywords
- graphene
- preparation
- graphite
- eps
- alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- 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
- C08J9/12—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 by a physical blowing agent
- C08J9/14—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 by a physical blowing agent organic
- C08J9/141—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
- C08J9/20—Making expandable particles by suspension polymerisation in the presence of the blowing agent
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- 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
-
- 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
-
- 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
- C08K9/00—Use of pretreated ingredients
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
Abstract
The present invention relates to a kind of preparation method of graphene and the preparations of graphene EPS:Intercalation is carried out to graphite with oxidation intercalator, High power microwavs continuous swelling is carried out to this intercalated graphite and ultrasound is removed, few layer graphene is prepared, the graphene is modified, then it is polymerize again with styrene monomer, the graphene EPS moulding articles prepared after foaming can reach anti-static effect, and mechanical property also obtains larger raising.Graphene prepared by the present invention, dispersant graft is good in styrene monomer, has given full play to that graphene conductive is good and mechanical characteristic, can play a significant role in specific areas such as military project, electric power.The sheet resistance of graphene EPS moulding articles produced by the present invention is up to 106~1012Ω, tensile strength reach B1 grades up to 0.7 1.0Mpa, compression strength up to 0.35 0.45Mpa, flame retardant rating.
Description
Technical field
The present invention relates to graphene preparation, graphene modification and graphene applied technical field, more particularly, to a kind of stone
The preparation method of black alkene and its preparation method of graphene EPS.
Background technology
Graphene be it is a kind of by the tightly packed two dimensional crystal material formed of carbon atom, it is excellent because it has unique structure
The performances such as different electricity, mechanics, optics, chemistry and calorifics become the hot spot of many people research.
The downstream application of graphene is not always up to expection, especially in field of compound material.Graphene preparation has redox
Method and Physical etc., graphene is because of large specific surface area, and usual reactivity is all higher, the graphene side especially after redox
Edge can also be left some active groups or inhibition group, so graphene should carry out appropriate modification, graphite before downstream application
The modification of alkene is related to change, grafting or surface package of group etc., and therefore, the modification of graphene is preparation and the downstream of graphene
Critically important one ring of centre in.
At present, in the method for graphene preparation of industrialization, the production capacity that Physical prepares graphene is limited, and is generally all existed
Ton/year, and the graphene stability produced is poor, and oxidation-reduction method prepares graphene process stabilizing, yield is higher, generally may be used
Up to 100 tons/year, it is suitble to a kind of preparation method of large-scale production, but the post processing cost of the spent acid after its redox is higher,
It is the principal element that cost can not be greatly lowered in graphene.
Oxidation-reduction method, which prepares graphene, mainly Brodie methods, Staudenmaier methods, Hummers methods, improvement
Hummers methods etc., Brodie methods, Staudenmaier methods are containing concentrated nitric acid, KClO3System can have been generated in reaction process
Poisonous gas and pollution it is more serious.Existing Hummers methods are improved in Hummers methods, are the concentrated sulfuric acid, nitrate, potassium permanganate body
System, 98% concentrated sulfuric acid are generally the 30-90 (mass ratio, similarly hereinafter) of graphite, and nitrate is the 1-5 of graphite, and potassium permanganate is graphite
1-10, while to use other strong oxidizers, such as hydrogen peroxide, hydrochloric acid, Strong oxdiative intercalator usage amount is big, seriously polluted;
Simultaneously in order to which reaction process is controlled to stablize, generally want first ice bath or step up thermotonus again after being reacted in low temperature;
In actual large-scale production process, Strong oxdiative intercalator usage amount can increase oxidation-reduction method, and post processing cost is high, pollution is big, and
Real reaction activity is more difficult to control, and technology stability is poor, danger coefficient is big.It is few to be badly in need of a kind of oxidation intercalator dosage of exploitation,
The good graphene preparation method of technology stability.
EPS, that is, expandable polystyrene adds in foaming agent using polystyrene resin beads, while heating is softened,
Gas is generated, forms a kind of foamed plastics of rigid closed cell structure, EPS is mainly used in the packaging of product food, external wall
The fields such as heat preservation, but EPS product mechanical strengths are relatively low at present, limit the application of EPS manufactured goods, and in Militaryl package and electricity
The fields such as power, heavy industry, automobile, and antistatic field is needed, antistatic graphene EPS comes into being.
The content of the invention
The purpose of the present invention is that in view of the above shortcomings of the prior art, provides a kind of few layer of graphite of suboxides system
The manufacturing cost of graphene is greatly reduced in the preparation method of alkene, and environmentally friendly cost is greatly reduced.
It is a further object of the present invention to provide a kind of graphene method of modifying of suitable graphene industrialization downstream application, are
The industrial applications of graphene provide a kind of reliable way method.
It is a further object of the present invention to provide a kind of high intensity, high fire-retardance, anlistatig graphene EPS beads preparation side
Method and moulding article.
Technical scheme is as follows:
A kind of preparation method of graphene and its preparation of graphene EPS, comprise the following steps:
(1) the oxidation intercalation of graphite:Using the graphite of 50~200 mesh grain sizes as raw material, purity is more than 99%, by graphite and oxygen
Change intercalator mixing and carry out intercalation, the oxidation intercalator is acid, nitrate, the mixture of potassium permanganate, and mass ratio is graphite:
Acid:Nitrate:Potassium permanganate=1:1~5:0.1~0.5:0.1~0.5;
(2) high-frequency microwave continuous swelling prepares graphene:915MHz high-frequency microwaves carry out continuous swelling 20 to intercalated graphite
~200S controls 100~200KW of output power, and simple ultrasound is carried out after discharging and is removed into few layer graphene, the number of plies is 3~5
Layer;
(3) alcohol of graphene washes modification:The graphene that step (2) obtains is mixed to the matter of 1~5h, graphene and alcohol with alcohol
Amount is than being 1:5~10, it carries out alcohol and washes modified filtration drying;
(4) preparation of graphene EPS:As needed for following suspension polymerization system prepared by raw material and its mass percent:
Preferably, the acid is the concentrated sulfuric acid that mass fraction is 90%-98%.
Preferably, the nitrate is at least one of sodium nitrate, potassium nitrate.
Preferably, the alcohol is at least one of methanol, ethyl alcohol, n-butanol, normal propyl alcohol.
Preferably, the initiator is dibenzoyl peroxide, peroxidized t-butyl perbenzoate, peroxide acetic acid butyl ester
At least one of.
Preferably, the dispersant is active calcium phosphate.
Preferably, the dispersion aids is at least one of sodium sulphate, sodium hydrogensulfite, magnesium carbonate, talcum powder.
The preparation process of the graphene EPS is:
A, the graphene that obtains mass percent styrene, pure water, step (3), dispersant, are added to dispersion aids
In reaction kettle, 10~20min of pre-dispersed stirring is carried out, mixing speed keeps 100-150r/min;
B, and then initiator is added in, mixing speed keeps 150-200r/min, and starts to warm up;When material in reactor temperature
When degree rises to 88~91 DEG C, when polymerisation 6~8 is small at this temperature;
C, seal pot tank adds foaming agent pentane, continues to heat up;When material in reactor temperature rises to 115~125 DEG C
When, when constant temperature holding 3.5~6 is small;
D, after hot stage, decrease temperature and pressure takes out material filtering, then dry graphene EPS beads;Finally,
Foaming is prepared into various graphene EPS moulding articles.
The present invention is beneficial to be had technical effect that:
(1) a kind of preparation method method of new graphene is developed, graphene preparation technology route is ripe, is suitble to industry
Change big production;(2) preparation of this graphene significantly reduces the cost of existing preparation of industrialization and environmentally friendly cost;(3) provide
One kind is suitable for industrialized graphene method of modifying, and a kind of reliable way method is provided for the industrial applications of graphene;
(4) a kind of high intensity, high fire-retardance, the preparation method of anlistatig graphene EPS beads and moulding article (5) are provided in military bag
The fields such as dress and electric power, heavy industry, automobile, and antistatic field is needed, provide a kind of antistatic graphene EPS moulding article materials
Material;(6) the downstream application scope of graphene and the application range of graphene EPS have been widened.
Graphene through the applicant prepare and it is modified, polymerize with EPS made of graphene EPS moulding articles, can more carry
High graphene EPS product property indices, as high strength, high fire-retardance, it is antistatic the advantages that.This antistatic graphene
EPS moulding articles density is 20~25kg/m3, sheet resistance is up to 106~1012Ω, tensile strength reach 0.7-1.0Mpa, pressure resistance
Degree reaches B1 grades, can be applied to the fields such as Militaryl package and electric power, heavy industry, automobile, and need to prevent up to 0.35-0.45Mpa, flame retardant rating
Electrostatic art.
Description of the drawings
Fig. 1 is the tensile strength figure for the graphene EPS that the embodiment of the present invention 1~4 is prepared;
Fig. 2 is the compression strength figure for the graphene EPS that the embodiment of the present invention 1~4 is prepared.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is specifically described.
Embodiment 1
(1) the oxidation intercalation of graphite:Using the graphite of 50 mesh grain sizes as raw material, purity 99%, by graphite and oxidation intercalator
Mixing carries out intercalation, and oxidation intercalator system is the 90wt% concentrated sulfuric acids, sodium nitrate, potassium permanganate system, and mass ratio is graphite:It is dense
Sulfuric acid:Sodium nitrate:Potassium permanganate=1:1:0.1:0.1;
(2) high-frequency microwave continuous swelling prepares graphene:915MHz high-frequency microwaves carry out continuous swelling to intercalated graphite
20S controls output power 200KW, and simple ultrasound is carried out after discharging and is removed into few layer graphene, and the number of plies is at 3~5 layers, specific surface
Product 1500m2/ g, lamellar spacing 0.8-3nm;
(3) alcohol of graphene washes modification:By graphene and a certain amount of ethyl alcohol mixing 1h, the mass ratio of graphene and ethyl alcohol
For 1:5, it carries out alcohol and washes modified filtration drying;
(4) preparation of graphene EPS:Raw material needed for suspension polymerization system and its mass percent are:
It concretely comprises the following steps:
A, by mass percent styrene 30%, pure water 66.75%, modified graphene 0.25%, active calcium phosphate
0.4%th, talcum powder 0.05%, be added in reaction kettle, carry out pre-dispersed stirring 10min, mixing speed keeps 100r/min;
B, and then dibenzoyl peroxide 0.05% is added in, mixing speed keeps 150r/min, and starts to warm up;Work as reaction
When material temperature in kettle rises to 91 DEG C, when polymerisation 6 is small at this temperature;
C, seal pot tank adds foaming agent pentane 2.5%, continues to heat up;When material in reactor temperature rises to 125 DEG C
When, when constant temperature holding 3.5 is small;
D, after hot stage, decrease temperature and pressure takes out material filtering, then dry graphene EPS beads;Finally,
Foaming is prepared into various graphene EPS moulding articles.
This antistatic graphene EPS moulding articles density is 20kg/m3, sheet resistance is up to 1012Ω, tensile strength reach
0.7Mpa, compression strength reach 0.35Mpa, and flame retardant rating reaches B1 grades.
Embodiment 2
(1) the oxidation intercalation of graphite:Using the graphite of 100 mesh grain sizes as raw material, purity 99.5%, by graphite and oxidation intercalation
Agent mixing carries out intercalation, and oxidation intercalator system is the 98wt% concentrated sulfuric acids, sodium nitrate, potassium nitrate, potassium permanganate system, mass ratio
For graphite:The concentrated sulfuric acid:Sodium nitrate:Potassium nitrate:Potassium permanganate=1:5:0.2:0.3:0.5;
(2) high-frequency microwave continuous swelling prepares graphene:915MHz high-frequency microwaves carry out continuous swelling to intercalated graphite
200S controls output power 100KW, and simple ultrasound is carried out after discharging and is removed into few layer graphene, and the number of plies is at 3~5 layers, specific surface
Product 2100m2/ g, lamellar spacing 0.8-3nm;
(3) alcohol of graphene washes modification:By graphene and a certain amount of methanol, ethyl alcohol mixing 5h, graphene and methanol, second
The mass ratio of alcohol is 1:5:5, it carries out alcohol and washes modified filtration drying;
(4) preparation of graphene EPS:Raw material needed for suspension polymerization system and its mass percent are:
It concretely comprises the following steps:
A, by mass percent styrene 35%, pure water 59.05%, modified graphene 0.65%, active calcium phosphate
1%th, sodium sulphate 0.05%, magnesium carbonate 0.05%, be added in reaction kettle, carry out pre-dispersed stirring 20min, mixing speed is kept
150r/min;
B, and then peroxide acetic acid butyl ester 0.2% is added in, mixing speed keeps 200r/min, and starts to warm up;When anti-
When answering the material temperature in kettle to rise to 88 DEG C, when polymerisation 8 is small at this temperature;
C, seal pot tank adds foaming agent pentane 4%, continues to heat up;When material in reactor temperature rises to 115 DEG C,
When constant temperature holding 6 is small;
D, after hot stage, decrease temperature and pressure takes out material filtering, then dry graphene EPS beads;Finally,
Foaming is prepared into various graphene EPS moulding articles.
Antistatic graphene EPS moulding articles density is 25kg/m3, sheet resistance is up to 106Ω, tensile strength reach 0.8Mpa,
Compression strength reaches 0.38Mpa, flame retardant rating reaches B1 grades.
Embodiment 3
(1) the oxidation intercalation of graphite:Using the graphite of 150 mesh grain sizes as raw material, purity 99.8%, by graphite and oxidation intercalation
Agent mixing carries out intercalation, and oxidation intercalator system is the 93wt% concentrated sulfuric acids, potassium nitrate, potassium permanganate system, and mass ratio is graphite:
The concentrated sulfuric acid:Potassium nitrate:Potassium permanganate=1:2:0.2:0.2;
(2) high-frequency microwave continuous swelling prepares graphene:915MHz high-frequency microwaves carry out continuous swelling to intercalated graphite
120S controls output power 120KW, and simple ultrasound is carried out after discharging and is removed into few layer graphene, and the number of plies is at 3~5 layers, specific surface
Product 1700m2/ g, lamellar spacing 0.8-3nm;
(3) alcohol of graphene washes modification:By graphene and a certain amount of ethyl alcohol, n-butanol mixing 2h, graphene and ethyl alcohol,
The mass ratio of n-butanol is 1:2:4, it carries out alcohol and washes modified filtration drying;
(4) preparation of graphene EPS:Raw material needed for suspension polymerization system and its mass percent are:
It concretely comprises the following steps:
A, by mass percent styrene 32%, pure water 63.83%, modified graphene 0.4%, active calcium phosphate
0.6%th, sodium sulphate 0.04%, sodium hydrogensulfite 0.03%, be added in reaction kettle, carry out pre-dispersed stirring 16min, stirring speed
Degree keeps 125r/min;
B, and then dibenzoyl peroxide 0.05%, peroxidized t-butyl perbenzoate 0.05% are added in, mixing speed is kept
170r/min, and start to warm up;When material in reactor temperature rises to 89 DEG C, when polymerisation 7 is small at this temperature;
C, seal pot tank adds foaming agent pentane 3%, continues to heat up;When material in reactor temperature rises to 119 DEG C,
When constant temperature holding 4.5 is small;
D, after hot stage, decrease temperature and pressure takes out material filtering, then dry graphene EPS beads;Finally,
Foaming is prepared into various graphene EPS moulding articles.
This antistatic graphene EPS moulding articles density is 22kg/m3, sheet resistance is up to 1010Ω, tensile strength reach
1.0Mpa, compression strength reach B1 grades up to 0.45Mpa flame retardant ratings.
Embodiment 4
(1) the oxidation intercalation of graphite:Using the graphite of 200 mesh grain sizes as raw material, purity 99.9%, by graphite and oxidation intercalation
Agent mixing carries out intercalation, and oxidation intercalator system is the 95wt% concentrated sulfuric acids, potassium nitrate, potassium permanganate system, and mass ratio is graphite:
The concentrated sulfuric acid:Nitrate:Potassium permanganate=1:4:0.4:0.4;
(2) high-frequency microwave continuous swelling prepares graphene:915MHz high-frequency microwaves carry out continuous swelling to intercalated graphite
85S controls output power 150KW, and simple ultrasound is carried out after discharging and is removed into few layer graphene, and the number of plies is at 3~5 layers, specific surface
Product 1950m2/ g, lamellar spacing 0.8-3nm;
(3) alcohol of graphene washes modification:By graphene and a certain amount of normal propyl alcohol mixing 3h, the matter of graphene and normal propyl alcohol
Amount is than being 1:8, it carries out alcohol and washes modified filtration drying;
(4) preparation of graphene EPS:Raw material needed for suspension polymerization system and its mass percent are:
It concretely comprises the following steps:
A, by mass percent styrene 34%, pure water 60.92%, modified graphene 0.55%, active calcium phosphate
0.8%th, sodium sulphate 0.08%, be added in reaction kettle, carry out pre-dispersed stirring 17min, mixing speed keeps 135r/min;
B, and then peroxidized t-butyl perbenzoate 0.05%, peroxide acetic acid butyl ester 0.1% are added in, mixing speed is kept
185r/min, and start to warm up;When material in reactor temperature rises to 90 DEG C, when polymerisation 7.5 is small at this temperature;
C, seal pot tank adds foaming agent pentane 3.5%, continues to heat up;When material in reactor temperature rises to 122 DEG C
When, when constant temperature holding 5.5 is small;
D, after hot stage, decrease temperature and pressure takes out material filtering, then dry graphene EPS beads;Finally,
Foaming is prepared into various graphene EPS moulding articles.
This antistatic graphene EPS moulding articles density is 23kg/m3, sheet resistance is up to 108Ω, tensile strength reach
0.9Mpa, compression strength reach 0.42Mpa, and flame retardant rating reaches B1 grades.
Test case:
1st, the tensile strength for the graphene EPS that Examples 1 to 4 is prepared and compression strength figure be as depicted in figs. 1 and 2.
2nd, the graphene prepared in embodiment 3 is subjected to the stone prepared after reaction kettle polymerize with commercially available graphene XFQ021
The performance of black alkene EPS moulding articles is compared, and polymerization technique, graphene EPS moulding article preparation processes are all in embodiment 3
Preparation process.The results are shown in Table 1.
Table 1
Claims (8)
1. a kind of preparation method of graphene EPS, it is characterised in that comprise the following steps:
(1) the oxidation intercalation of graphite:Using the graphite of 50~200 mesh grain sizes as raw material, purity is more than 99%, and graphite and oxidation are inserted
Layer agent mixing carries out intercalation, and the oxidation intercalator is acid, nitrate, the mixture of potassium permanganate, and mass ratio is graphite:Acid:
Nitrate:Potassium permanganate=1:1~5:0.1~0.5:0.1~0.5;
(2) high-frequency microwave continuous swelling prepares graphene:915MHz high-frequency microwaves to intercalated graphite carry out continuous swelling 20~
200S controls 100~200KW of output power, and ultrasound is carried out after discharging and is removed into few layer graphene, the number of plies is at 3~5 layers;
(3) alcohol of graphene washes modification:The graphene that step (2) obtains is mixed to the mass ratio of 1~5h, graphene and alcohol with alcohol
For 1:5~10, it carries out alcohol and washes modified filtration drying;
(4) preparation of graphene EPS:As needed for following suspension polymerization system prepared by raw material and its mass percent:
2. preparation method according to claim 1, it is characterised in that the acid is the dense sulphur that mass fraction is 90%-98%
Acid.
3. preparation method according to claim 1, it is characterised in that the nitrate for sodium nitrate, in potassium nitrate at least
It is a kind of.
4. preparation method according to claim 1, it is characterised in that the alcohol is methanol, in ethyl alcohol, n-butanol, normal propyl alcohol
At least one.
5. preparation method according to claim 1, it is characterised in that the initiator is dibenzoyl peroxide, peroxidating
At least one of t-butyl perbenzoate, peroxide acetic acid butyl ester.
6. preparation method according to claim 1, it is characterised in that the dispersant is active calcium phosphate.
7. preparation method according to claim 1, it is characterised in that the dispersion aids for sodium sulphate, sodium hydrogensulfite,
At least one of magnesium carbonate, talcum powder.
8. preparation method according to claim 1, it is characterised in that the preparation process of the graphene EPS is:
A, the graphene that obtains mass percent styrene, pure water, step (3), dispersant, are added to reaction at dispersion aids
In kettle, 10~20min of pre-dispersed stirring is carried out, mixing speed keeps 100-150r/min;
B, and then initiator is added in, mixing speed keeps 150-200r/min, and starts to warm up;When material in reactor temperature liter
During to 88~91 DEG C, when polymerisation 6~8 is small at this temperature;
C, seal pot tank adds foaming agent pentane, continues to heat up;It is permanent when material in reactor temperature rises to 115~125 DEG C
When temperature holding 3.5~6 is small;
D, after hot stage, decrease temperature and pressure takes out material filtering, then dry graphene EPS beads;Finally, foam
It is prepared into various graphene EPS moulding articles.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711225261.3A CN108084306A (en) | 2017-11-29 | 2017-11-29 | A kind of preparation method of modified graphene and its application for preparing EPS |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711225261.3A CN108084306A (en) | 2017-11-29 | 2017-11-29 | A kind of preparation method of modified graphene and its application for preparing EPS |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108084306A true CN108084306A (en) | 2018-05-29 |
Family
ID=62173332
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201711225261.3A Pending CN108084306A (en) | 2017-11-29 | 2017-11-29 | A kind of preparation method of modified graphene and its application for preparing EPS |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108084306A (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102583351A (en) * | 2012-02-29 | 2012-07-18 | 中国科学院宁波材料技术与工程研究所 | Preparation method of fewer-layer graphene |
CN106188608A (en) * | 2016-07-25 | 2016-12-07 | 江苏利士德化工有限公司 | A kind of method of the expandable polystyrene particles of preparation of industrialization graphene-containing |
CN106752116A (en) * | 2016-11-15 | 2017-05-31 | 吉林省云亭节能技术有限公司 | The preparation method and modified graphene oxide EPS of modified graphene oxide mold the preparation method of styrofoam |
-
2017
- 2017-11-29 CN CN201711225261.3A patent/CN108084306A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102583351A (en) * | 2012-02-29 | 2012-07-18 | 中国科学院宁波材料技术与工程研究所 | Preparation method of fewer-layer graphene |
CN106188608A (en) * | 2016-07-25 | 2016-12-07 | 江苏利士德化工有限公司 | A kind of method of the expandable polystyrene particles of preparation of industrialization graphene-containing |
CN106752116A (en) * | 2016-11-15 | 2017-05-31 | 吉林省云亭节能技术有限公司 | The preparation method and modified graphene oxide EPS of modified graphene oxide mold the preparation method of styrofoam |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP4903037B2 (en) | Expandable vinyl aromatic polymers and methods for their preparation | |
CN105732860B (en) | The expandable polystyrene bead and preparation method of inflatable few layer graphene | |
CN114163712B (en) | Graphene composite PE material and preparation method thereof | |
CN104141259B (en) | A kind of environment-friendly type cation phenylpropyl surface sizing agent and preparation method thereof | |
CN107987410B (en) | Preparation of graphene EPS master batch and EPS compounding method | |
CN106188608B (en) | A kind of method of the expandable polystyrene particles of preparation of industrialization containing graphene | |
CN108084307A (en) | A kind of preparation method of graphene and its method of static conductive graphene EPS | |
JPH02284905A (en) | Foaming olefinic resin particles modified with carbon-containing styrene | |
CN106674783A (en) | Preparation method of high-strength graphene expandable polystyrene board | |
CN110229372A (en) | Low molding energy consumption polypropylene foamed particles of one kind and preparation method thereof | |
CN108084306A (en) | A kind of preparation method of modified graphene and its application for preparing EPS | |
CN105602114A (en) | Polypropylene foamed composite board and manufacturing method thereof | |
CN102838710B (en) | Novel polypropylene graft-modification method | |
CN102382222A (en) | Low-density polyethylene (LDPE) resin for cable insulant having voltage level of above 110kV, and preparation method thereof | |
CN107141384B (en) | Production method of high-blackness graphite expandable polystyrene particles | |
CN1080293A (en) | The production method of expandable styrene-polymer spheres | |
CN106661423A (en) | Gas-Generating Agent, And Process For Producing Foamed Object Using Same | |
WO2014111628A2 (en) | Method of producing polystyrene beads having low moisture content | |
JPH0554854B2 (en) | ||
CN108084583A (en) | A kind of preparation method of graphene and its preparation of sound insulation graphene EPS | |
JPH0598062A (en) | Foamable styrene resin granule and production thereof | |
JPS6213442A (en) | Production of carbon-containing expandable styrene resin particle | |
CN107459671A (en) | A kind of modified expanded microballoon for polypropylene plastics foaming and preparation method thereof | |
CN103923382A (en) | Foamed polypropylene bead with low melting point and high cementability and preparation method thereof | |
CN113444280B (en) | Preparation method of organic intercalated hydrotalcite modified expandable polystyrene beads |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180529 |