CN102166866A - Method for preparing antistatic laminated material from graphene - Google Patents
Method for preparing antistatic laminated material from graphene Download PDFInfo
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- CN102166866A CN102166866A CN2011100007793A CN201110000779A CN102166866A CN 102166866 A CN102166866 A CN 102166866A CN 2011100007793 A CN2011100007793 A CN 2011100007793A CN 201110000779 A CN201110000779 A CN 201110000779A CN 102166866 A CN102166866 A CN 102166866A
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Abstract
The invention relates to a method for preparing an antistatic laminated material from graphene, in particular to a method for preparing an antistatic laminated material from graphene in a novel nano-structure. The method comprises the following steps of: carrying out ultrasonic treatment on the mixed liquid of graphite and a solvent to prepare graphene uniform dispersion liquid; carrying out condensation polymerization between melamine and formaldehyde to obtain melamine-formaldehyde resin; uniformly mixing the graphene uniform dispersion liquid and the melamine-formaldehyde resin under the condition of stirring to form a conductive melamine-formaldehyde resin adhesive; fully soaking paper for a decorative board in the prepared antistatic melamine-formaldehyde resin adhesive; regularly laminating the dried paper soaked with resin; and combining the paper with other layers under the conditions of heating and pressing to form a laminated board. In the invention, by adding the graphene dispersion liquid into the melamine-formaldehyde resin, the surface resistance of a resin decorative laminated board reaches 105 ohms, and the surface resistance of a pure melamine-formaldehyde resin decorative laminated board reaches up to 1012-1014 ohms.
Description
Technical field
The Graphene that the present invention relates to use the novel nano structure prepares the method for antistatic lamination material, refers in particular to Graphene is applied in the anlistatig carbamide pre-polymerization resin class laminated material of preparation aspect.
Background technology
Melamine formaldehyde resin has that glue-joint strength height, curing rate are fast, water-fast, heat-resisting, wear-resisting, resistance to chemical attack, nontoxic, excellent properties such as put out certainly, extensive use is wood adhesive, wet strength agent for papermaking, leather composite tanning agent, coating, textile finshing agent, power engineering plastics, impregnating agent etc.But the electrical insulation capability of this resin is very good, and its resistance value is generally up to 10
12～10
14 Ω, in processing and use, be very easy to producing static, and be not easy to disappear, gathering in a large number of electric charge can cause electrostatic hazard, gently then hinders packing, dust suction, also can produce in the time of seriously to catch fire and accident such as blast; In addition, melamine formaldehyde resin cured glue layer easily breaks, fragility is strong, is difficult for moving and packing.Want to enlarge the range of application of melamine formaldehyde resin, improve its application quality, just must eliminate its electrostatic interaction, improve its fragility, reduce it and break.
In order to eliminate the electrostatic interaction of melamine formaldehyde resin material, adding antistatic additive is the effective ways that reduce this resin material sheet resistance, makes the rapid discharge of resin material can prevent gathering of static by the sheet resistance that reduces resin.At present, the antistatic additive that uses both at home and abroad mainly is that surfactant type antistatic additive, carbon are filler antistatic additive, metal species filler antistatic additive etc.
The surfactant type antistatic additive generally is brushing in the synthetic or process at resin material, is sprayed on product surface, by the hydrone in the hydrophilic group absorbed air of antistatic additive, with formation layer of surface conducting film, thereby eliminate the static that produces, belong to external application type antistatic additive.The major advantage of external application type antistatic additive is that consumption is little, instant effect, but be difficult to realize even coating, be subjected to the influence of air humidity bigger, antistatic effect is very poor when air humidity is lower than 50%, and take off mistake because of friction, washing easily, antistatic poor durability can only provide antistatic effect temporary transient or short-term.Simultaneously, the dust in its also easy absorbed air and the surrounding environment, particle etc. cause ion or chemical contamination, and form outward appearance greasy, that stain at product surface.
Metal species filler antistatic additive comprises metal, metal oxide, slaine etc.For example,, cost an arm and a leg though metal conductive powder electric conductivity such as nickel, copper and chromium are strong, poor with the performed polymer compatibility, can cause the mechanical properties decrease of institute's goods more obvious, and then influence elasticity, the flexibility of institute's prepared material, its limitation is arranged when using.
Carbon is filler antistatic additive such as conductive black, graphite granule, carbon fiber, this type of antistatic additive good stability, cheap, difficult dispersion and loading are big in colloid, disperse inhomogeneous meeting to cause the antistatic property on institute goods surface inhomogeneous, and high filler loading capacity can make poor processability, reduced the mechanical property of composite, cause antistatic particle to come off, resistivity is wayward, and reappearance is relatively poor etc.
Weak point at above antistatic additive existence, the inventor finds, recent the novel nano-material----Graphene of finding, have excellent electricity, mechanical property, it is the highest material of intensity on the present the known world, compare few, the good dispersion of its addition with other conductive filler antistatic additive; Compare with the surfactant type antistatic additive, it can conform well, good stability, and improved to a certain extent resin material fragility, reduced it and broken.The adding of solvent has significantly reduced the viscosity of resin in the process that is mixed, and has improved the permeability of resin, is very suitable for developing the laminated material of high-antistatic performance, is a march toward important directions of practical application of graphene nano material.
Summary of the invention
The object of the present invention is to provide Graphene with the novel nano structure to be doped in the melamine formaldehyde resin eliminating the electrostatic hazard that is brought in this resin application process, thereby make this resin satisfy the demand of different field.
Technical scheme of the present invention is: use the method that novel nano structure Graphene prepares antistatic lamination material.It is characterized in that: the mixed liquor of graphite and solvent is carried out ultrasonic, make the equal dispersion liquid of Graphene; Melamine becomes melamine formaldehyde resin with formaldehyde condensation polymer; Under stirring condition, the Graphene dispersion liquid is added in the carbamide pre-polymerization resin, mix, form antistatic melamine formaldehyde resin glue, decorative panel is fully flooded in made antistatic melamine formaldehyde resin glue with paper, to be soaked with the ply of paper folded neat (determining the number of plies) of resin, drying again, under heating and pressure, it be combined with sandwich layer, form laminate by decorative panel thickness.
The present invention includes following steps:
(1) graphite is mixed by a certain percentage with solvent, it is standby to make the Graphene dispersion liquid through ultrasonic processing;
(2) with melamine and formaldehyde according to molar feed ratio 1:2.5, it is standby to form melamine formaldehyde resins 80 ℃ of following polycondensations, wherein said formaldehyde is that mass fraction is 37% formalin;
(3) step (1) gained Graphene dispersion liquid is added in step (2) the gained resin by a certain percentage, stir evenly and promptly make antistatic carbamide pre-polymerization resin glue, the mass ratio of wherein said Graphene and melamine formaldehyde resin is 1/16000～1/160;
(3) decoration veneer that will be cut into the certain size size impregnated in the antistatic melamine formaldehyde resin glue with ph test paper ph, treats that every paper all takes out behind the more than enough resin of immersion foot, drips unnecessary resin;
(4) ph test paper ph that will soak glue is put into vacuum drying chamber in 80～140 ℃ of oven dry down;
(5) ph test paper ph with oven dry takes out, and repeating step (3), (4) are once again;
(6) ph test paper ph that has soaked antistatic melamine formaldehyde resin glue is stacked neat, be covered on the sandwich layer, place on the smooth aluminium alloy plate, in 135 ℃, 0.5～10.3MPa is heating 15min down, promptly makes anlistatig laminate on hydraulic press.
Wherein the graphite described in the step (1) is graphite powder or natural flake graphite; Wherein said solvent be 37% formalin,
N, N-dimethyl formamide (DMF),
NIn-methyl pyrrolidone (NMP), acetone, methyl alcohol, the ethanol one or more; The ultrasonic power of wherein said ultrasonic processing is 250w; The thickness of wherein said Graphene is 5～10nm, is of a size of 100nm
2～100 μ m
2The mass ratio of wherein said Graphene and solvent is 1/200～1/57.
The present invention compared with prior art, its remarkable advantage is: the face resistance of the melamine formaldehyde resin of the Graphene that mixed is by original 10
12～10
14 ΩDrop to 10
5 Ω, eliminated the electrostatic hazard that this resin is in use brought, improved its application quality.
Description of drawings
Accompanying drawing 1 is the schematic flow sheet that using mineral carbon alkene of the present invention prepares the method for antistatic lamination material.
The specific embodiment
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
Among the present invention made decoration veneer is carried out the face resistance test.The method of testing of face resistance is megger test method (referring to a GB-T4677.1-1984-printed board top layer megger test method).
Embodiment 1
(1) preparation of the equal dispersion liquid of Graphene
The 0.5g graphite powder is added among the 40.0gNMP, and ultrasonic 6h under 250w makes the equal dispersion liquid of NMP of Graphene.
(2) preparation of carbamide pre-polymerization resin
Polycondensation reaction is taken place with molar feed ratio 1:2.5 in melamine and formaldehyde, forms precipitation, be little muddiness, illustrate and precipitate than reaching 1:1 as if mixture than in 1mL distilled water, slowly splashing into the 1mL naval stores for 1:1() the carbamide pre-polymerization resin.
(3) preparation of antistatic veener plate
(thickness of Graphene is 5～10nm, is of a size of 100nm with the equal dispersion liquid of the described 4.9g Graphene of step (1)
2～100 μ m
2) and 10g carbamide pre-polymerization resin directly mix, stir and promptly make antistatic carbamide pre-polymerization resin glue.The decoration veneer of a 3.0cm * 3.0cm be impregnated in the antistatic carbamide pre-polymerization resin glue with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make the antistatic layer pressing plate, survey its face resistance with the megger test method, experimental result sees Table 1.
Embodiment 2
(1) preparation of the equal dispersion liquid of Graphene
The 0.5g natural flake graphite is added among the 40.0gNMP, and ultrasonic 6h under 250w makes the equal dispersion liquid of NMP of Graphene.
(2) preparation of carbamide pre-polymerization resin
Polycondensation reaction is taken place with molar feed ratio 1:2.5 in melamine and formaldehyde, forms precipitation, be little muddiness, illustrate and precipitate than reaching 1:1 as if mixture than in 1mL distilled water, slowly splashing into the 1mL naval stores for 1:1() the carbamide pre-polymerization resin.
(3) preparation of antistatic veener plate
(thickness of Graphene is 5～10nm, is of a size of 100nm with the equal dispersion liquid of the described 4.9g Graphene of step (1)
2～100 μ m
2) and 10g carbamide pre-polymerization resin directly mix, stir and promptly make antistatic carbamide pre-polymerization resin glue.The decoration veneer of a 3.0cm * 3.0cm be impregnated in the antistatic carbamide pre-polymerization resin glue with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make the antistatic layer pressing plate, survey its face resistance with the megger test method, experimental result sees Table 1.
Embodiment 3
(1) preparation of the equal dispersion liquid of Graphene
The 0.4g graphite powder is added among the 40.0gNMP, and ultrasonic 6h under 250w makes the equal dispersion liquid of NMP of Graphene.
(2) preparation of carbamide pre-polymerization resin
Polycondensation reaction is taken place with molar feed ratio 1:2.5 in melamine and formaldehyde, forms precipitation, be little muddiness, illustrate and precipitate than reaching 1:1 as if mixture than in 1mL distilled water, slowly splashing into the 1mL naval stores for 1:1() the carbamide pre-polymerization resin.
(3) preparation of antistatic veener plate
(thickness of Graphene is 5～10nm, is of a size of 100nm with the equal dispersion liquid of the described 6.1g Graphene of step (1)
2～100 μ m
2) and 10g carbamide pre-polymerization resin directly mix, stir and promptly make antistatic carbamide pre-polymerization resin glue.The decoration veneer of a 3.0cm * 3.0cm be impregnated in the antistatic carbamide pre-polymerization resin glue with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make the antistatic layer pressing plate, survey its face resistance with the megger test method, experimental result sees Table 1.
Embodiment 4
(1) preparation of the equal dispersion liquid of Graphene
The 0.5g graphite powder is added among the 40.0gDMF, and ultrasonic 6h under 250w makes the equal dispersion liquid of DMF of Graphene.
(2) preparation of carbamide pre-polymerization resin
Polycondensation reaction is taken place with molar feed ratio 1:2.5 in melamine and formaldehyde, forms precipitation, be little muddiness, illustrate and precipitate than reaching 1:1 as if mixture than in 1mL distilled water, slowly splashing into the 1mL naval stores for 1:1() the carbamide pre-polymerization resin.
(3) preparation of antistatic veener plate
(thickness of Graphene is 5～10nm, is of a size of 100nm with the equal dispersion liquid of the described 4.9g Graphene of step (1)
2～100 μ m
2) and 10g carbamide pre-polymerization resin directly mix, stir and promptly make antistatic carbamide pre-polymerization resin glue.The decoration veneer of a 3.0cm * 3.0cm be impregnated in the antistatic carbamide pre-polymerization resin glue with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make the antistatic layer pressing plate, survey its face resistance with the megger test method, experimental result sees Table 1.
Embodiment 5
(1) preparation of the equal dispersion liquid of Graphene
The 0.3g graphite powder is added in the 43.0g formalin, and ultrasonic 6h under 250w makes the equal dispersion liquid of formalin of Graphene.
(2) preparation of antistatic veener plate
The 26.7g melamine is added in the equal dispersion liquid of formalin of step (1) gained Graphene, 80 ℃ polycondensation reaction takes place down, when reaction pre-assemble adhesive precipitation slowly splashes into the 1mL naval stores than reaching 1:1(in 1mL distilled water, if mixture is little muddiness, illustrate that precipitation is than reaching 1:1) time, to react glue pours in the clean surface ware, again the decoration veneer of a 3.0cm * 3.0cm be impregnated in the antistatic pre-polymerization resin glue with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, the decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make the antistatic layer pressing plate, survey its face resistance with the megger test method, experimental result sees Table 1.
Embodiment 6
(1) preparation of the equal dispersion liquid of Graphene
The 0.5g graphite powder is added among the 40.0gNMP, and ultrasonic 6h under 250w makes the equal dispersion liquid of NMP of Graphene.
(2) preparation of carbamide pre-polymerization resin
Polycondensation reaction is taken place with molar feed ratio 1:2.5 in melamine and formaldehyde, forms precipitation, be little muddiness, illustrate and precipitate than reaching 1:1 as if mixture than in 1mL distilled water, slowly splashing into the 1mL naval stores for 1:1() the carbamide pre-polymerization resin.
(3) preparation of antistatic veener plate
(thickness of Graphene is 5～10nm, is of a size of 100nm with the equal dispersion liquid of the described 4.1g Graphene of step (1)
2～100 μ m
2) and 10g carbamide pre-polymerization resin directly mix, stir and promptly make antistatic carbamide pre-polymerization resin glue.The decoration veneer of a 3.0cm * 3.0cm be impregnated in the antistatic carbamide pre-polymerization resin glue with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make the antistatic layer pressing plate, survey its face resistance with the megger test method, experimental result sees Table 1.
Reference examples
(1) preparation of carbamide pre-polymerization resin
Polycondensation reaction is taken place with molar feed ratio 1:2.5 in melamine and formaldehyde, forms precipitation, be little muddiness, illustrate and precipitate than reaching 1:1 as if mixture than in 1mL distilled water, slowly splashing into the 1mL naval stores for 1:1() the carbamide pre-polymerization resin.
(2) preparation of thick china
4.9gNMP and 10g carbamide pre-polymerization resin are directly mixed, and stirring promptly makes colloidal pitch.The decoration veneer of a 3.0cm * 3.0cm be impregnated in the colloidal resin with paper, wait to decorate and take out after thick china has flooded abundant resin with paper, drip unnecessary resin, put into the vacuum drying chamber oven dry, temperature is controlled at (80～140) ℃, oven dry, decoration veneer behind the impregnation is stacked and place on the smooth aluminium alloy plate with paper and same size polytetrafluoroethylplastic plastic, on hydraulic press in 135 ℃, 10MPa is heating 15min down, promptly make laminate, survey its face resistance with the megger test method, experimental result sees Table 1.
Table 1
| The experiment number | Resistance/ Ω |
| Embodiment 1 | 3.6×10 5 |
| Embodiment 2 | 5.8×10 5 |
| Embodiment 3 | 4.2×10 5 |
| Embodiment 4 | 8.0×10 5 |
| Embodiment 5 | 9.2×10 5 |
| Embodiment 6 | 3.3×10 6 |
| Reference examples | 3.0×10 12 |
The present invention utilizes the good electric conductivity of nano-graphene by add the method for Graphene in melamine formaldehyde resin, and the face resistance that makes the pre-polymerization resin decorative laminate is by original 3.0 * 10
12 ΩDrop to 10
5～10
6 Ω, make product have good antistatic performance, the application quality that this has improved product has greatly enlarged its range of application.
Claims (2)
1. using mineral carbon alkene prepares the method for antistatic lamination material, it is characterized in that carrying out according to following step:
(1) graphite is mixed by a certain percentage with solvent, it is standby to make the Graphene dispersion liquid through ultrasonic processing;
(2) with melamine and formaldehyde according to molar feed ratio 1:2.5, it is standby to form melamine formaldehyde resins 80 ℃ of following polycondensations, wherein said formaldehyde is that mass fraction is 37% formalin;
(3) step (1) gained Graphene dispersion liquid is added in step (2) the gained resin by a certain percentage, stir evenly and promptly make antistatic carbamide pre-polymerization resin glue, the mass ratio of wherein said Graphene and melamine formaldehyde resin is 1/16000～1/160;
(3) decoration veneer that will be cut into the certain size size impregnated in the antistatic melamine formaldehyde resin glue with ph test paper ph, treats that every paper all takes out behind the more than enough resin of immersion foot, drips unnecessary resin;
(4) ph test paper ph that will soak glue is put into vacuum drying chamber in 80～140 ℃ of oven dry down;
(5) ph test paper ph with oven dry takes out, and repeating step (3), (4) are once again;
(6) ph test paper ph that has soaked antistatic melamine formaldehyde resin glue is stacked neat, be covered on the sandwich layer, place on the smooth aluminium alloy plate, in 135 ℃, 0.5～10.3MPa is heating 15min down, promptly makes anlistatig laminate on hydraulic press.
2. using mineral carbon alkene according to claim 1 prepares the method for antistatic lamination material, it is characterized in that wherein the graphite described in the step (1) is graphite powder or natural flake graphite; Wherein said solvent be 37% formalin,
N, N-dimethyl formamide (DMF),
NIn-methyl pyrrolidone (NMP), acetone, methyl alcohol, the ethanol one or more; The ultrasonic power of wherein said ultrasonic processing is 250w; The thickness of wherein said Graphene is 5～10nm, is of a size of 100nm
2～100 μ m
2The mass ratio of wherein said Graphene and solvent is 1/200～1/57.
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| CN103554861A (en) * | 2013-11-04 | 2014-02-05 | 哈尔滨市都邦节能科技有限公司 | Graphene high polymer plate as well as preparation method thereof |
| CN104203577A (en) * | 2012-04-03 | 2014-12-10 | 索尼公司 | Laminated structure manufacturing method, laminated structure, and electronic apparatus |
| CN105646809A (en) * | 2016-01-12 | 2016-06-08 | 浙江新华新材料科技有限责任公司 | Graphene amino resin preparation method and device |
| CN108177410A (en) * | 2017-12-30 | 2018-06-19 | 郑州峰泰纳米材料有限公司 | A kind of composite bed melamine bubble silk floss and preparation method thereof |
| CN108248178A (en) * | 2018-01-25 | 2018-07-06 | 上海君江科技有限公司 | A kind of melamine faced chipboard of antistatic and preparation method thereof |
| CN108951271A (en) * | 2018-08-17 | 2018-12-07 | 枣庄市天龙纸业有限公司 | A kind of novel environment friendly facing paper and preparation method thereof |
| CN113233918A (en) * | 2021-04-27 | 2021-08-10 | 常州中复丽宝第复合材料有限公司 | Light heat-preservation high-toughness fireproof plate and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102557023A (en) * | 2012-03-12 | 2012-07-11 | 大连丽昌新材料有限公司 | Method for preparing graphene |
| CN104203577A (en) * | 2012-04-03 | 2014-12-10 | 索尼公司 | Laminated structure manufacturing method, laminated structure, and electronic apparatus |
| CN103554861A (en) * | 2013-11-04 | 2014-02-05 | 哈尔滨市都邦节能科技有限公司 | Graphene high polymer plate as well as preparation method thereof |
| CN103554861B (en) * | 2013-11-04 | 2015-09-09 | 哈尔滨市都邦节能科技有限公司 | A kind of preparation method of Graphene polymer sheet material |
| CN105646809A (en) * | 2016-01-12 | 2016-06-08 | 浙江新华新材料科技有限责任公司 | Graphene amino resin preparation method and device |
| CN108177410A (en) * | 2017-12-30 | 2018-06-19 | 郑州峰泰纳米材料有限公司 | A kind of composite bed melamine bubble silk floss and preparation method thereof |
| CN108248178A (en) * | 2018-01-25 | 2018-07-06 | 上海君江科技有限公司 | A kind of melamine faced chipboard of antistatic and preparation method thereof |
| CN108951271A (en) * | 2018-08-17 | 2018-12-07 | 枣庄市天龙纸业有限公司 | A kind of novel environment friendly facing paper and preparation method thereof |
| CN113233918A (en) * | 2021-04-27 | 2021-08-10 | 常州中复丽宝第复合材料有限公司 | Light heat-preservation high-toughness fireproof plate and preparation method thereof |
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Application publication date: 20110831 |