CN108912653A - The preparation method of graphene/waterborne polyurethane conductive composite material for civilian leather and its preparation method of graphene dispersing solution - Google Patents
The preparation method of graphene/waterborne polyurethane conductive composite material for civilian leather and its preparation method of graphene dispersing solution Download PDFInfo
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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
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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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
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- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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Abstract
The invention discloses the preparation methods of the graphene/waterborne polyurethane conductive composite material for civilian leather, by 100 parts of aqueous polyurethane in parts by weight, 1-4 parts of graphene dispersing solution, 2-8 parts of water cross-linking agent, 0.05-0.1 parts of aqueous levelling agent, 0.2-1 parts of aqueous defoamer, aqueous hand feeling agent 0.3-3 parts, 0.5-5 parts of thickener be uniformly mixed, grinding, filtering after to get to for civilian leather graphene/waterborne polyurethane conductive composite material.Graphene dispersing solution is prepared by the following method：It improves Hummer method and prepares graphite oxide；In aqueous solution by graphite oxide and polyvinylpyrrolidone dispersion；Graphene oxide is reduced into graphene by heat-treating.Preparation process of the invention is brief environmentally friendly, efficient, and especially suitable for multiple qualities such as sofa artificial leather, massage armchair leather, luggage leather, clothing leathers, not only class sense is strong but also durable, has the very strong market competitiveness.
Description
Technical field
The present invention relates to artificial leather material field, the graphene/waterborne polyurethane conduction of more particularly, to civilian leather is multiple
The preparation method of condensation material and its preparation method of graphene dispersing solution.
Background technique
Property possessed by leather and feel, in the decoration for becoming luggage, clothes, shoes, vehicle and furniture
The synonym of " top grade " has sufficiently obtained the affirmative in market, and application range is wide, and quantity is big, as many as kind, it is difficult to estimate
Amount.And since the natural leather production cycle is long, limited amount, artificial leather becomes its substitute, and also type is numerous in artificial leather field
More, high-grade artificial leather is even also more expensive than corium price.
Synthetic Leather by the development of many years with its good appearance feel and breathable moisture permeability, wear-resisting solvent resistant,
It high-intensitive, many advantages, such as being widely used, is widely applied in the fields such as industrial, civilian, military, production with people,
It lives closely bound up.
Waterborne polyurethane resin has hardness is high, adhesive force is strong, corrosion-resistant, solvent resistant, volatile organic content are low etc.
Advantage, at the same also have many advantages, such as it is nontoxic, non-ignitable, free from environmental pollution and energy saving, in crosslinking agent, packaging material and coating row
Industry has good development prospect, but the thermal stability compared to organic solvent polyurethane, solvent resistance and mechanical property etc. are all
Therefore popularization and application that are lower, directly affecting for the comprehensive performance of raising, need to carry out it to be rationally effectively modified,
Currently, mainly crosslinking modification, the acrylic acid extremely modification, epoxy resin modification, organic-silicon-modified of the cruel method of modifying of aqueous poly- ammonia
And inorganic nano material modified etc. and inorganic nano material（SiO2、TiO2, CNTs etc.）Because its size is small, large specific surface area, make
Obtaining nanocomposite has superior physical property and mechanical property compared with conventional composites materials.
Graphene was irrigated from 2004 by Univ Manchester UK physicist An Deliegaimu and Constantine's promise
Xiao Luofu isolates graphene with micromechanics stripping method success from graphite, therefore obtains Nobel's physics in 2010 jointly
Prize.It is exactly graphite that graphene gathers into folds from level to level, and thick 1 millimeter of graphite comprises about 3,000,000 layers of graphene, grapheme material
Theoretical specific surface area is up to 2600m2/g；Heating conduction（3000W /m·K）；The carrier mobility of graphene at room temperature is about
For 15000cm/ (Vs), this numerical value has been more than 10 times of silicon materials；The theoretical Young's modulus of graphene reaches 1.0TPa, inherently
Tensile strength be 130GPa.
The common preparation method of graphene is micromechanics stripping method, oxidation-reduction method, SiC epitaxial growth method, liquid phase method, change
Oxidation-reduction method etc. is learned, film production method is chemical vapour deposition technique (CVD).Each method has the advantage and disadvantage of oneself：
Micromechanics removing is only suitable for laboratory research, and epitaxial growth method and Chemical Vapor Deposition Equipment are expensive, liquid phase method production effect
Rate is low；Chemistry redox method is a kind of important method, its advantage is that it is at low cost, high-efficient, the disadvantage is that product graphene has
Defect, area are small etc., and intermediate product graphite oxide needs to restore can just obtain graphene.
The method restored at present mainly has thermal reduction and electronation；Thermal reduction is quickly to heat graphite oxide（>
2000℃/min）To 1050 DEG C, graphite oxide is made to generate CO between layers under nitrogen protection2Gas, it is swollen by gas
It is swollen that limellar stripping is opened；Electronation hair is restored using chemical method, and chemical reagent used has hydrazine, Dimethylhydrazine, to hexichol
Phenol, NaBH4Deng；Using the suspension of hydrazine reduced graphene oxide serving, the graphene nanoplatelets of reunion can be made, after dry
Conductive black powder is obtained, conductivity is about 200Sm-1, but graphite ene product is easily reunited under van der Waals interaction, is
Overcoming reunion of the graphene in reduction process, reducing agent or aggregation can be added in researcher in graphene oxide,
Then electronation again, the graphene aqueous solution of the available gelatinous chemical modification of homogeneous.
Summary of the invention
Goal of the invention：Above-mentioned to solve the problems, such as, the purpose of the present invention is to provide a kind of graphene/aqueous poly- ammonia
The preparation method of ester conducing composite material.Using the special single layer of graphene, two-dimensional nanostructure, height is hard, transparent, conductive, leads
The properties such as heat increase substantially the antistatic effect of civilian leather, wear-resisting scratch resistance performance.The second is being replaced using aqueous polyurethane
For traditional solvent borne polyurethane, organic solvent pollution is eliminated from source, is eliminated safe hidden trouble, operating personnel's building ring is improved
Border, ecological, environmental protective.Preparation process is simple and efficient, pollution-free.
Summary of the invention：The preparation method of graphene/waterborne polyurethane conductive composite material for civilian leather, will be with weight
100 parts of aqueous polyurethane of part meter, 1-4 parts of graphene dispersing solution, 2-8 parts of water cross-linking agent, 0.05-0.1 parts of aqueous levelling agent,
0.2-1 parts of aqueous defoamer, aqueous hand feeling agent 0.3-3 parts, 0.5-5 parts of thickener be uniformly mixed, grinding, after filtering to get arriving
Graphene/waterborne polyurethane conductive composite material for civilian leather.
Preferably, the aqueous polyurethane, be one of aqueous polyurethane of bloom, zero diopter or sub-smooth type or
A combination thereof.The aqueous polyurethane of bloom, zero diopter or sub-smooth type can bring up the special light sensation of automobile leather, embody class.
Further, the aqueous polyurethane includes one of aliphatic polyurethane, aromatic polyurethane or its group
It closes.Aliphatic and aromatic aqueous polyurethane respectively have feature, can be applicable in the leather surface processing of different demands.
Preferably, the graphene dispersing solution is graphene aqueous solution, the concentration of graphene is 2mg/ml ~ 5mg/ml.
The graphene dispersing solution uses aqueous solution, meets the objective of the invention for mainly using water-based material, environmentally protective, concentration and matter
The advantages of arrangement of amount number can make graphene in composition obtains maximum performance.
Preferably, the graphene/waterborne polyurethane conductive composite material, the civilian leather of application includes sofa artificial leather, presses
Rub chair leather, luggage leather, clothing leather.The application field of civilian leather is mostly to increase the field comfortably experienced, and allows the conducing composite material
It is grounded gas, can have excellent comprehensive performance, splendid use feeling is brought to consumer.
The formula constituent of the graphene/waterborne polyurethane conductive composite material, using 700 ~ 800r/ of high-speed mixer
Min is uniformly mixed.High-speed stirred ensure that mixture homogeneity, provide condition for subsequent coating.
The preparation method of the graphene dispersing solution of graphene/waterborne polyurethane conductive composite material for civilian leather, packet
Include following steps：
（1）, by improve Hummer method prepare graphite oxide；
（2）, by the graphite oxide prepared and polyvinylpyrrolidone dispersion in aqueous solution, obtain graphite oxide dispersion；
（3）, by heat-treating graphene oxide is reduced into graphene, obtain graphene dispersing solution.The stone obtained using the method
Black alkene dispersion liquid quality is high, and application is wide, is suitable for and other component compatibilities.
Compared to the prior art, the beneficial effects of the present invention are：Graphene for civilian leather of the invention/aqueous poly-
The preparation method of urethane conducing composite material and its preparation method of graphene dispersing solution, formula is reasonable, simple process, and function is strong
Greatly.Using the special single layer of graphene, two-dimensional nanostructure, the properties such as height is hard, transparent, conductive, thermally conductive are increased substantially
The wear-resisting scratch resistance performance of automobile leather；Traditional solvent borne polyurethane is substituted using aqueous polyurethane, eliminates organic solvent from source
Pollution, eliminates safe hidden trouble, and improves operating personnel's working environment, ecological, environmental protective；To propose the market competitiveness of civilian leather；It utilizes
Polyvinylpyrrolidone auxiliary, improves the dispersibility and stability of high concentration graphene aqueous solution, and using simple and environmentally-friendly molten
Liquid complex method prepares composite material.Preparation process of the invention is brief environmentally friendly, efficient, especially suitable for sofa artificial leather, massage armchair
Multiple qualities such as leather, luggage leather, clothing leather, not only class sense is strong but also durable, has the very strong market competitiveness.
Specific embodiment
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, letter will be made to embodiment below
Single introduction.
A kind of preparation method of graphene/waterborne polyurethane conductive composite material, by aqueous polyurethane in parts by weight
100 parts, 1-4 parts of graphene dispersing solution, 2-8 parts of water cross-linking agent, 0.05-0.1 parts of aqueous levelling agent, aqueous defoamer 0.2-1
Part, aqueous hand feeling agent 0.3-3 part, 0.5-5 part of thickener be uniformly mixed, grinding, filtering after to get arrive be used for civilian leather graphite
Alkene/waterborne polyurethane conductive composite material；
Wherein, the aqueous polyurethane is one of aqueous polyurethane of bloom, zero diopter or sub-smooth type or a combination thereof,
It and include one of aliphatic polyurethane, aromatic polyurethane or combinations thereof；The graphene dispersing solution is graphene
Aqueous solution, the concentration of graphene are 2mg/ml ~ 5mg/ml；
Wherein, the preparation method of the graphene dispersing solution of the conducing composite material, includes the following steps：
（1）, by improve Hummer method prepare graphite oxide；
（2）, by the graphite oxide prepared and polyvinylpyrrolidone dispersion in aqueous solution, obtain graphite oxide dispersion；
（3）, by heat-treating graphene oxide is reduced into graphene, obtain graphene dispersing solution.
The civilian leather of application includes the fields such as sofa artificial leather, massage armchair leather, luggage leather, clothing leather.
Embodiment is used below, and specific preparation process and parameter are introduced：
Embodiment 1
The preparation of graphene dispersing solution, the preparation of graphene/waterborne polyurethane conductive composite material, include the following steps：
（1）, graphite oxide preparation：Using Hummer method is improved, by natural flake graphite, dense H2SO4And NaNO3Mixture
KMnO is added in middle gradation4, 0-10 DEG C of reaction temperature, after being stirred to react 5h is controlled, is washed product in HCl and distilled water
Property, it is dry, obtain graphite oxide；
（2）, 2mg/ml graphene aqueous solution preparation：320mg graphite oxide and 480mg polyvinylpyrrolidone is taken to be added to
In 160ml deionized water, it is ultrasonically treated 5min, 1ml ammonium hydroxide, then ultrasound 5min is added, after graphite oxide aqueous dispersion, dress
Enter autoclave, is heated to 170 DEG C, is taken out after saturated vapour pressure 8MPa, 12h, obtain graphene aqueous solution, concentration 2mg/ml；
（3）, graphene/waterborne polyurethane conductive composite material preparation：Take 33.33g solid content be 30% aqueous polyurethane with
50ml's（2）Obtained graphene aqueous solution is poured into beaker, and the water cross-linking agent, aqueous being added according to weight metering ratio is carried
Levelling agent, aqueous defoamer, aqueous hand feeling agent, thickener, mixing, stir 30min, mixing speed under conditions of 25 DEG C
700r/min, grinding, filtering decontamination, is made conducing composite material.
After conducing composite material is made, it is coated in base fabric：
Conducing composite material is uniformly applied in base fabric, speed is 9 ~ 11m/min, and coating layer thickness is controlled in 0.15 ~ 0.3mm range
It is interior, aqueous polyurethane layer is made；The combination of aqueous polyurethane layer and base fabric is strong after drying, not easily to fall off, and aqueous poly- ammonia
Ester layer elasticity is good, and cortex is soft, has good feel, and antistatic effect greatly enhances.
Obtained aqueous polyurethane layer heats 30min at 50 DEG C, and the conductivity for measuring sample is 2.94 × 10-5S/cm。
Embodiment 2
The preparation of graphene dispersing solution, the preparation of graphene/waterborne polyurethane conductive composite material, include the following steps：
（1）, graphite oxide preparation：Using Hummer method is improved, by natural flake graphite, dense H2SO4And NaNO3Mixture
KMnO is added in middle gradation4, 0-10 DEG C of reaction temperature, after being stirred to react 5h is controlled, is washed product in HCl and distilled water
Property, it is dry, obtain graphite oxide；
（2）, 2mg/ml graphene aqueous solution preparation：320mg graphite oxide and 1280mg polyvinylpyrrolidone is taken to be added to
In 160ml deionized water, it is ultrasonically treated 5min, 1ml ammonium hydroxide, then ultrasound 5min is added, after graphite oxide aqueous dispersion, dress
Enter autoclave, is heated to 160 DEG C, is taken out after saturated vapour pressure 7MPa, 5h, obtain graphene aqueous solution, concentration 2mg/ml；
（3）, graphene/waterborne polyurethane conductive composite material preparation：Take 33.33g solid content be 30% aqueous polyurethane with
200ml's（2）Obtained graphene aqueous solution is poured into beaker, and water cross-linking agent, the water being added according to weight metering ratio are carried
Property levelling agent, aqueous defoamer, aqueous hand feeling agent, thickener, mixing, stir 30min under conditions of 25 DEG C, mixing speed
800r/min, grinding, filtering decontamination, is made conducing composite material.
After conducing composite material is made, it is coated in base fabric：
Conducing composite material is uniformly applied in base fabric, speed is 9 ~ 11m/min, and coating layer thickness is controlled in 0.15 ~ 0.3mm range
It is interior, aqueous polyurethane layer is made；The combination of aqueous polyurethane layer and base fabric is strong after drying, not easily to fall off, and aqueous poly- ammonia
Ester layer elasticity is good, and cortex is soft, has good feel, and antistatic effect greatly enhances.
Obtained aqueous polyurethane layer heats 30min at 50 DEG C, and the conductivity for measuring sample is 8.3 × 10-4S/cm。
Embodiment 3
The preparation of graphene dispersing solution, the preparation of graphene/waterborne polyurethane conductive composite material, include the following steps：
（1）, graphite oxide preparation：Using Hummer method is improved, by natural flake graphite, dense H2SO4And NaNO3Mixture
KMnO is added in middle gradation4, 0-10 DEG C of reaction temperature, after being stirred to react 5h is controlled, is washed product in HCl and distilled water
Property, it is dry, obtain graphite oxide；
（2）, 4mg/ml graphene aqueous solution preparation：640mg graphite oxide and 960mg polyvinylpyrrolidone is taken to be added to
In 160ml deionized water, it is ultrasonically treated 5min, 1ml ammonium hydroxide, then ultrasound 5min is added, after graphite oxide aqueous dispersion, dress
Enter autoclave, is heated to 150 DEG C, is taken out after saturated vapour pressure 7MPa, 8h, obtain graphene aqueous solution, concentration 4mg/ml；
（3）, graphene/waterborne polyurethane conductive composite material preparation：Take 33.33g solid content be 30% aqueous polyurethane with
100ml's（2）Obtained graphene aqueous solution is poured into beaker, and water cross-linking agent, the water being added according to weight metering ratio are carried
Property levelling agent, aqueous defoamer, aqueous hand feeling agent, thickener, mixing, stir 30min under conditions of 25 DEG C, mixing speed
750r/min, grinding, filtering decontamination, is made conducing composite material.
After conducing composite material is made, it is coated in base fabric：
Conducing composite material is uniformly applied in base fabric, speed is 9 ~ 11m/min, and coating layer thickness is controlled in 0.15 ~ 0.3mm range
It is interior, aqueous polyurethane layer is made；The combination of aqueous polyurethane layer and base fabric is strong after drying, not easily to fall off, and aqueous poly- ammonia
Ester layer elasticity is good, and cortex is soft, has good feel, and antistatic effect greatly enhances.
Obtained aqueous polyurethane layer heats 30min at 50 DEG C, and the conductivity for measuring sample is 1.24 × 10-4S/cm。
Above embodiments are only to illustrate the preferred technical solution of the present invention, it is noted that for the common skill of the art
For art personnel, without departing from the principle of the present invention, several improvement made or equivalent replacement are accordingly to be regarded as the present invention
Protection scope, should cover within the scope of the claims of the present invention.
Claims (7)
1. the preparation method of the graphene/waterborne polyurethane conductive composite material for civilian leather, which is characterized in that will be with weight
100 parts of aqueous polyurethane of part meter, 1-4 parts of graphene dispersing solution, 2-8 parts of water cross-linking agent, 0.05-0.1 parts of aqueous levelling agent,
0.2-1 parts of aqueous defoamer, aqueous hand feeling agent 0.3-3 parts, 0.5-5 parts of thickener be uniformly mixed, grinding, after filtering to get arriving
Graphene/waterborne polyurethane conductive composite material for civilian leather.
2. the preparation method of the graphene/waterborne polyurethane conductive composite material according to claim 1 for civilian leather,
It is characterized in that, the aqueous polyurethane, is one of aqueous polyurethane of bloom, zero diopter or sub-smooth type or its group
It closes.
3. the preparation method of the graphene/waterborne polyurethane conductive composite material according to claim 2 for civilian leather,
It is characterized in that, the aqueous polyurethane, includes one of aliphatic polyurethane, aromatic polyurethane or combinations thereof.
4. the preparation method of the graphene/waterborne polyurethane conductive composite material according to claim 1 for civilian leather,
It is characterized in that, the graphene dispersing solution is graphene aqueous solution, the concentration of graphene is 2mg/ml ~ 5mg/ml.
5. the preparation method of the graphene/waterborne polyurethane conductive composite material according to claim 1 for civilian leather,
It is characterized in that, the graphene/waterborne polyurethane conductive composite material, the civilian leather of application include sofa artificial leather, massage armchair leather,
Luggage leather, clothing leather.
6. the preparation method of the graphene/waterborne polyurethane conductive composite material according to claim 1 for civilian leather,
The formula constituent of the graphene/waterborne polyurethane conductive composite material is stirred mixed using 700 ~ 800r/min of high-speed mixer
It closes uniform.
7. described in any item graphene/waterborne polyurethane conductive composite materials for civilian leather according to claim 1 ~ 6
The preparation method of graphene dispersing solution, which is characterized in that include the following steps：
（1）, by improve Hummer method prepare graphite oxide；
（2）, by the graphite oxide prepared and polyvinylpyrrolidone dispersion in aqueous solution, obtain graphite oxide dispersion；
（3）, by heat-treating graphene oxide is reduced into graphene, obtain graphene dispersing solution.
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Citations (5)
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|---|---|---|---|---|
| CN102093700A (en) * | 2010-12-30 | 2011-06-15 | 常州大学 | Method for preparing graphene/waterborne polyurethane conductive composite material |
| CN105297449A (en) * | 2015-07-30 | 2016-02-03 | 四川大学 | Waterborne wear-resistant and scraping-resistant surface treating agent for artificial leather and synthetic leather and preparation method |
| CN105696367A (en) * | 2014-11-25 | 2016-06-22 | 佛山市高明区生产力促进中心 | Polyurethane artificial leather and making method thereof |
| CN105926308A (en) * | 2016-05-12 | 2016-09-07 | 宋婷婷 | Formula and technology for producing synthetic leather from graphene modified waterborne polyurethane |
| CN106948183A (en) * | 2017-02-28 | 2017-07-14 | 佛山市高明威仕达塑料有限公司 | A kind of super abrasive aqueous coating PVC leather and processing technology |
-
2018
- 2018-07-18 CN CN201810790125.7A patent/CN108912653A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102093700A (en) * | 2010-12-30 | 2011-06-15 | 常州大学 | Method for preparing graphene/waterborne polyurethane conductive composite material |
| CN105696367A (en) * | 2014-11-25 | 2016-06-22 | 佛山市高明区生产力促进中心 | Polyurethane artificial leather and making method thereof |
| CN105297449A (en) * | 2015-07-30 | 2016-02-03 | 四川大学 | Waterborne wear-resistant and scraping-resistant surface treating agent for artificial leather and synthetic leather and preparation method |
| CN105926308A (en) * | 2016-05-12 | 2016-09-07 | 宋婷婷 | Formula and technology for producing synthetic leather from graphene modified waterborne polyurethane |
| CN106948183A (en) * | 2017-02-28 | 2017-07-14 | 佛山市高明威仕达塑料有限公司 | A kind of super abrasive aqueous coating PVC leather and processing technology |
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Application publication date: 20181130 |