CN109721269A - A method of preparing graphene-plant fiber compound - Google Patents
A method of preparing graphene-plant fiber compound Download PDFInfo
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- CN109721269A CN109721269A CN201910150510.XA CN201910150510A CN109721269A CN 109721269 A CN109721269 A CN 109721269A CN 201910150510 A CN201910150510 A CN 201910150510A CN 109721269 A CN109721269 A CN 109721269A
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- plant fiber
- graphene oxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The invention belongs to building material technical field, discloses and a kind of prepare graphene-plant fiber compound method.It comprises the following steps that: 1 preparation graphene oxide dispersion；2 pairs of natural plant fibres carry out pre-treatment；3 immerse plant fiber in certain density graphene oxide dispersion, and drying is taken out after full penetration；4 will restore in graphene oxide-plant fiber immersion reducing solution, and graphene-plant fiber compound is obtained after drying.The process flow is simple to operation, and the graphene film of plant fibre surface cladding can hinder the erosion of cement matrix neutral and alkali ion pair plant fiber as protective film, improves fiber durability, has very big application prospect in terms of cement-based material is split in toughening resistance.
Description
Technical field
The present invention relates to the methods for coating one layer of graphene in plant fibre surface, belong to building material technical field.
Background technique
Cement-based material is current construction material most commonly used in the world, but it be fragile material, it is easy to crack.Research
Show that fiber has good control action to the cracking of cement-based material.Steel fibre and artificial synthetic fiber to a certain extent can
The toughness of concrete is improved, but improves the cost of concrete.For the cost that fiber concrete is effectively reduced, researcher starts
Using distributed in nature is extensive, cheap, the convenient plant fiber of materials replaces traditional artificial synthetic fiber.Plant
Fiber applications can not only improve toughness in cement-base composite material, additionally it is possible to and it promotes sustainable development, there is ecological effect,
Meet the Major Strategic developed a circular economy.
Endurance issues of the plant fiber in cement-base composite material limit it in the application of the field of building materials.Water
The calcium hydroxide that muddy waterization generates is soluble in water, makes cement slurry hole solution in alkalinity.Alkaline environment can make in plant fiber
Hemicellulose and lignin liquor, the structure for destroying fiber make the intensity and toughness decline of fiber.In addition, calcium ion enters plant
The crystallization of fibrous inside hole, makes fiber " mineralising ", gradually loses flexible and stiffening, Yi Fasheng brittle fracture.Therefore, it solves to plant
Endurance issues of the fibres in cement matrix are that plant fiber is replaced artificial synthetic fiber toughening cement-base composite material
Precondition.
Summary of the invention
In view of the above technical problems existing in the prior art, graphene-plant is prepared the object of the present invention is to provide a kind of
The method of fibre composites.This method will be dispersed in the graphene oxide layer packet in water using plant fiber porous water-absorbing characteristic
Plant fibre surface is overlayed on, stable graphene-plant fiber compound is obtained in reducing environment.Plant fibre surface packet
The graphene film covered can be used as the protective film of plant fiber, effectively hinder invading for cement matrix neutral and alkali ion pair plant fiber
Erosion improves durability of the plant fiber in cement matrix.The process flow is simple to operation, is expected to huge construction program and is applied to green
Building trade.
In order to achieve the above object, graphene-plant fiber compound method is prepared the present invention provides a kind of, it should
Method includes following procedure:
1) prepares graphene oxide, and configures graphene oxide water solution；
2) carries out pre-treatment to plant fiber；
3) immerses the plant fiber after pre-treatment in graphene oxide water solution, after full penetration, takes out drying and obtains
Graphene oxide-plant fiber compound；
4) immerses graphene oxide-plant fiber compound in reducing solution, obtains stable graphene-plant
Fibres compound.
In the step 1), graphene oxide, the graphene oxide water solution concentration of configuration are prepared with Hummers method is improved
For 1~3mg/ml.
In the step 2), the pre-treatment of plant fiber includes: 1. to be determined according to the requirement of toughening cement-base composite material
Plant fiber draw ratio range, and plant fiber is cut；2. cleaning soil, the clast etc. of plant fibre surface with clear water
Sundries, and dry；3. water washed plant fiber is impregnated 0.5~1h in the pH NaOH for being 13~14 or KOH solution, remove
The pectin and wax on surface expose more multi-surface；4. being dried after the plant fiber clear extremely neutrality of clear water after alkali process.
In the step 3), in order to promote graphene oxide to enter plant fiber hole, ultrasound is opened in soaking process
Oscillation, power are 300~600W.
In the step 3), drying course are as follows: the graphene oxide of taking-up-plant fiber compound is placed on gauze
Excessive moisture is drained, is dried in a vacuum drying oven, temperature is 40~60 DEG C.
In the step 4), the reducing solution be one of sodium borohydride, sodium ascorbate, concentration be 0.1~
3mol/L, reduction temperature are 40~80 DEG C.
The invention has the following beneficial effects: will be dispersed in the graphite oxide in water using plant fiber porous water-absorbing characteristic
Alkene lamella is coated on plant fibre surface, and stable graphene-plant fiber compound is obtained in reducing environment.The technique
Process is simple to operation, and the graphene of fiber surface package hinders cement matrix neutral and alkali ion as the protective film of plant fiber
Erosion to plant fiber improves plant fiber durability, can be applied to toughening cement-base composite material.
Detailed description of the invention
Fig. 1 is the Raman spectrum of sisal fiber after pre-treatment in the embodiment of the present invention；
Fig. 2 is graphene oxide-sisal fiber compound Raman spectrum in the embodiment of the present invention；
Fig. 3 is graphene-sisal fiber compound Raman spectrum in the embodiment of the present invention.
Specific embodiment
In order to illustrate more clearly of technical solution of the present invention, it is illustrated below in conjunction with specific embodiments and the drawings,
It should be evident that the embodiment in being described below is only some embodiments of the present invention, those of ordinary skill in the art are come
It says, without creative efforts, other examples can also be obtained according to these embodiments.
Embodiment 1 prepares graphene-sisal fiber compound by taking sisal fiber as an example.
(1) prepares graphene oxide with Hummers method is improved, and is configured to the graphene oxide water that concentration is 1mg/ml
Solution；
(2) pretreatment of sisal fiber: natural sisal fiber is cut into the staple fiber that length is 60mm, is washed with clear water
The silt particle and clast on surface, 60 DEG C of drying in blast drier.Then 1h is impregnated in 0.1mon/L NaOH solution.At alkali
Sisal fiber after reason spends clear water repeated flushing to neutrality, dries for 60 DEG C in blast drier.
(3) immerses the sisal fiber after pre-treatment in the graphene oxide water solution in step (1), sonic oscillation (function
Rate is 360W) 0.5h, after full penetration, takes out graphene oxide-sisal fiber, is placed on the gauze that mesh is 80 mesh and drains
Excessive moisture, it is sufficiently dry in 60 DEG C of vacuum oven to obtain graphene oxide-sisal fiber compound.
(4) immerses graphene oxide-sisal fiber in the sodium borohydride solution that concentration is 1mol/L, is placed in 70 DEG C
It is restored in water-bath, obtains graphene-sisal fiber compound.
Sisal fiber, graphene oxide-sisal fiber after being handled before being tested in above-mentioned preparation process with Raman spectrometer
Compound and graphene-sisal fiber compound Raman spectrum, as shown in Figs. 1-3.Wherein, in 1580cm-1Nearby occur
The peak G is as caused by the in plane vibration of carbon atom, is the principal character peak of graphene, in 1340cm-1The peak D nearby occurred is recognized
For the unordered vibration peak for being graphene.The provable graphene oxide of appearance at the peak D and the peak G is successfully coated on sisal fiber surface.
Embodiment 2 prepares graphene-sisal fiber compound by taking sisal fiber as an example.
(1) prepares graphene oxide with Hummers method is improved, and is configured to the graphene oxide water that concentration is 2mg/ml
Solution；
(2) pretreatment of sisal fiber: natural sisal fiber is cut into the staple fiber that length is 30mm, is washed with clear water
The silt particle and clast on surface, 60 DEG C of drying in blast drier.Then 0.5h is impregnated in 1mol/L NaOH solution.At alkali
Sisal fiber after reason spends clear water repeated flushing to neutrality, dries for 60 DEG C in blast drier.
(3) immerses the sisal fiber after pre-treatment in the graphene oxide water solution in step (1), sonic oscillation (function
Rate is 600W) 0.5h, after full penetration, takes out graphene oxide-sisal fiber, is placed on the gauze that mesh is 80 mesh and drains
Excessive moisture, it is sufficiently dry in 60 DEG C of vacuum oven to obtain graphene oxide-sisal fiber compound.
(4) immerses graphene oxide-sisal fiber in the sodium ascorbate that concentration is 0.5mol/L, is placed in 80 DEG C
It is restored in water-bath, obtains graphene-sisal fiber compound.
Embodiment 3 prepares graphene oxide-coir fibre compound by taking coir fibre as an example.
(1) prepares graphene oxide with Hummers method is improved, and is configured to the graphene oxide water that concentration is 2mg/ml
Solution；
(2) pretreatment of coir fibre: natural coconut fiber is cut into the staple fiber that length is 20~30mm, with clear
The silt particle and clast for washing surface, 60 DEG C of drying in blast drier.Then it is impregnated in 0.5mol/L NaOH solution
0.5h.Coir fibre after alkali process spends clear water repeated flushing to neutrality, dries for 60 DEG C in blast drier.
(3) immerses the coir fibre after pre-treatment in the graphene oxide water solution in step (1), sonic oscillation (function
Rate is 360W) 0.5h, after full penetration, takes out graphene oxide-coir fibre, is placed on the gauze that mesh is 80 mesh and drains
Excessive moisture, it is sufficiently dry in 60 DEG C of vacuum oven to obtain graphene oxide-coir fibre compound.
(4) immerses graphene oxide-coir fibre in the sodium ascorbate that concentration is 0.5mol/L, is placed in 60 DEG C
It is restored in water-bath, obtains graphene-coir fibre compound.
Embodiment 4 prepares graphene oxide-coir fibre compound by taking coir fibre as an example.
(1) prepares graphene oxide with Hummers method is improved, and is configured to the graphene oxide water that concentration is 3mg/ml
Solution；
(2) pretreatment of coir fibre: natural coconut fiber is cut into the staple fiber that length is 10~20mm, with clear
The silt particle and clast for washing surface, 60 DEG C of drying in blast drier.Then it is impregnated in 0.1mol/L NaOH solution
0.5h.Coir fibre after alkali process spends clear water repeated flushing to neutrality, dries for 60 DEG C in blast drier.
(3) immerses the coir fibre after pre-treatment in the graphene oxide water solution in step (1), sonic oscillation (function
Rate is 600W) 20min, after full penetration, takes out graphene oxide-coir fibre, is placed on the gauze that mesh is 80 mesh and drains
Excessive moisture, it is sufficiently dry in 60 DEG C of vacuum oven to obtain graphene oxide-coir fibre compound.
(4) immerses graphene oxide-coir fibre in the sodium borohydride solution that concentration is 1mol/L, is placed in 70 DEG C
It is restored in water-bath, obtains graphene-coir fibre compound.
Embodiment 5
By taking sisal fiber as an example, graphene-sisal fiber compound is prepared.
(1) prepares graphene oxide with Hummers method is improved, and is configured to the graphene oxide water that concentration is 1mg/ml
Solution；
(2) pretreatment of sisal fiber: natural sisal fiber is cut into the staple fiber that length is 60mm, is washed with clear water
The silt particle and clast on surface, 60 DEG C of drying in blast drier.Then 1h is impregnated in 0.1mon/L NaOH solution.At alkali
Sisal fiber after reason spends clear water repeated flushing to neutrality, dries for 60 DEG C in blast drier.
(3) immerses the sisal fiber after pre-treatment in the graphene oxide water solution in step (1), sonic oscillation (function
Rate is 300W) 0.5h, after full penetration, takes out graphene oxide-sisal fiber, is placed on the gauze that mesh is 80 mesh and drains
Excessive moisture, it is sufficiently dry in 60 DEG C of vacuum oven to obtain graphene oxide-sisal fiber compound.
(4) immerses graphene oxide-sisal fiber in the sodium borohydride solution that concentration is 3mol/L, is placed in 40 DEG C
It is restored in water-bath, obtains graphene-sisal fiber compound.
Embodiment 6
By taking coir fibre as an example, graphene oxide-coir fibre compound is prepared.
(1) prepares graphene oxide with Hummers method is improved, and is configured to the graphene oxide water that concentration is 2mg/ml
Solution；
(2) pretreatment of coir fibre: natural coconut fiber is cut into the staple fiber that length is 20~30mm, with clear
The silt particle and clast for washing surface, 60 DEG C of drying in blast drier.Then it is impregnated in 0.5mol/L NaOH solution
0.5h.Coir fibre after alkali process spends clear water repeated flushing to neutrality, dries for 60 DEG C in blast drier.
(3) immerses the coir fibre after pre-treatment in the graphene oxide water solution in step (1), sonic oscillation (function
Rate is 360W) 0.5h, after full penetration, takes out graphene oxide-coir fibre, is placed on the gauze that mesh is 80 mesh and drains
Excessive moisture, it is sufficiently dry in 40 DEG C of vacuum oven to obtain graphene oxide-coir fibre compound.
(4) immerses graphene oxide-coir fibre in the sodium ascorbate that concentration is 0.1mol/L, is placed in 60 DEG C
It is restored in water-bath, obtains graphene-coir fibre compound.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (6)
1. a kind of prepare graphene-plant fiber compound method, it is characterised in that: this method includes following procedure:
1) prepares graphene oxide, and configures graphene oxide water solution；
2) carries out pre-treatment to plant fiber；
3) immerses the plant fiber after pre-treatment in graphene oxide water solution, after full penetration, takes out drying and is aoxidized
Graphene-plant fiber compound；
4) immerses graphene oxide-plant fiber compound in reducing solution, and it is compound to obtain graphene-plant fiber
Object.
2. according to claim 1 prepare graphene-plant fiber compound method, it is characterised in that: the step
It is rapid 1) in, prepare graphene oxide with Hummers method is improved, the graphene oxide water solution concentration of configuration is 1~3mg/ml.
3. according to claim 1 prepare graphene-plant fiber compound method, which is characterized in that the step
It is rapid 2) in, the pre-treatment of plant fiber includes: 1. to determine plant fiber draw ratio according to the requirement of toughening cement-base composite material
Range, and plant fiber is cut；2. cleaning the sundries of plant fibre surface with clear water, and dry；3. by water washed
Plant fiber impregnates 0.5~1h in the pH NaOH for being 13~14 or KOH solution；4. the plant fiber clear water after alkali process is clear
It is dried after to neutrality.
4. according to claim 1 prepare graphene-plant fiber compound method, it is characterised in that: the step
It is rapid 3) in, open sonic oscillation in soaking process, power is 300~600W.
5. according to claim 1 prepare graphene-plant fiber compound method, it is characterised in that: the step
It is rapid 3) in, the detailed process of drying are as follows: the graphene oxide of taking-up-plant fiber compound is placed on gauze drain it is extra
Moisture is dried under vacuum conditions, and temperature is 40~60 DEG C.
6. according to claim 1 prepare graphene-plant fiber compound method, it is characterised in that: the step
It is rapid 4) in reducing solution be one of sodium borohydride, sodium ascorbate, concentration is 0.1~3mol/L, and reduction temperature is
40~80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910150510.XA CN109721269A (en) | 2019-02-28 | 2019-02-28 | A method of preparing graphene-plant fiber compound |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910150510.XA CN109721269A (en) | 2019-02-28 | 2019-02-28 | A method of preparing graphene-plant fiber compound |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138929A (en) * | 2020-01-13 | 2020-05-12 | 上海普合生态科技有限公司 | Nano composite graphene coating and preparation method thereof |
| CN112266260A (en) * | 2020-10-21 | 2021-01-26 | 安徽国风塑业股份有限公司 | Preparation method of polyimide graphite film |
-
2019
- 2019-02-28 CN CN201910150510.XA patent/CN109721269A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138929A (en) * | 2020-01-13 | 2020-05-12 | 上海普合生态科技有限公司 | Nano composite graphene coating and preparation method thereof |
| CN111138929B (en) * | 2020-01-13 | 2021-08-24 | 上海普合生态科技有限公司 | Nano composite graphene coating and preparation method thereof |
| CN112266260A (en) * | 2020-10-21 | 2021-01-26 | 安徽国风塑业股份有限公司 | Preparation method of polyimide graphite film |
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Application publication date: 20190507 |