CN104986982B - A kind of fire-retardant stalk material of graphene oxide and preparation method thereof - Google Patents
A kind of fire-retardant stalk material of graphene oxide and preparation method thereof Download PDFInfo
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- CN104986982B CN104986982B CN201510428513.7A CN201510428513A CN104986982B CN 104986982 B CN104986982 B CN 104986982B CN 201510428513 A CN201510428513 A CN 201510428513A CN 104986982 B CN104986982 B CN 104986982B
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- 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
Abstract
The present invention is to provide a kind of fire-retardant stalk material of graphene oxide and preparation method thereof.Stalk fibre is dried, by mechanical lapping to granularity below 100 μm；Graphene oxide is placed in ultrasonic disperse in deionized water and after 3 hours, obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml 1mg/ml.Stalk powder after mechanical grinding is poured in graphene oxide water solution and carries out ultrasonic disperse 30min；Will dispersion after mixed system stir under the conditions of 90 DEG C be evaporated to thick, and at 60 DEG C be dried remove remnants moisture, be coated with or the fire-retardant stalk compound material of graphene oxide of multilayer oxygen functionalized graphene.Preparation technology of the present invention is simple, environmental friendliness, provides new approach for exploitation straw application in building material field, has broad application prospects.
Description
Technical field:
The present invention relates to a kind of fire-retardant stalk material of graphene oxide and preparation method thereof, belong to fire protection flame retarding building
Field of material technology.
Background technology:
China is a large agricultural country, and stalk resource is the abundantest, and distribution is wide, kind is many and yield is huge.According to statistics,
China's agricultural crop straw annual production is 700,000,000 t, first of the row world, accounts for about the 30% of whole world straw total amount.According to investigations, at present
China's straw utilization rate is about 33%, and major part does not adds process, and utilize after technical finesse only accounts for about 2.6%.Straw
Main based on building block, sheet material in building material field application.But in application process, have that goods are inflammable, corrosion-resistant,
The problems such as added value is the highest.Therefore, develop straw new application, improve straw self performance, promote its added value, improve it in merit
The application of energy Material Field has practical significance.
Graphene is owing to having high-specific surface area, and excellent heat stability, electric property and mechanical property, at composite wood
The research in the fields such as material enhancing and conduction receives significant attention.In graphene nano material preparation process, graphene film interlayer
Van der Waals force often referred to as hinder the subject matter of graphene dispersion.If in building material field, we utilize stone
The heat stability of ink alkene excellence and the Van der Waals force of graphene film interlayer, prepare under conditions of being added without other modifying agent and have
The graphene oxide stalk compound material of core-shell structure, reaches under the state using less filler, and composite is substantially improved
Fire retardant performance, this development that will promote Novel fireproof flame-retardant material and progress.Compare the fire-retardant neck of traditional building material
Generally there is preparation technology in territory relative complex, fire retardant burning brings the problem of smoke toxicity, and the present invention has preparation technology letter
List, environmental protection, the advantage of nonhazardous.This research at home and abroad there is no report.
Summary of the invention:
It is an object of the invention to provide a kind of fire-retardant stalk material of graphene oxide and preparation method, technique is simple, cost
Cheap, environmental friendliness, it is possible to make inflammable straw become the material preparation method with fire resistance.
A kind of graphene oxide fire-retardant stalk material preparation method of the present invention, comprises the following steps:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 2-4 hour
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:(100 ~ 500) ratio of (g/ml) mix after ultrasonic disperse
10-30min；
4) described composite mechanical agitation at 80-90 DEG C is evaporated to mixture be thick after, at 50-60 DEG C
It is dried 12 hours, it is thus achieved that the stalk powder of graphene oxide coating.
Described straw is one or more mixing in corn straw, wheat stalk, rice straw, broomcorn straw
Thing.
The fire resistance of product of the present invention can reach B1 level.
The positive effect of the present invention is: with graphene oxide as modifying agent, realizes oxidation stone under spin coating evaporation technology
Ink alkene is in the coating of stalk powder particle surface, thus prepares the fire-retardant stalk material of graphene oxide.The theoretical foundation of the present invention
It is: owing to Graphene has high-specific surface area, excellent heat stability, stronger Van der Waals force, during solution evaporation
The concentration of graphene oxide constantly promotes, along with high-speed stirred, with stalk powder particle for reaction under physics chemical action
Center, it is achieved graphene oxide is in the attachment of straw particle surface.And owing to graphene film interlayer has stronger Van der Waals
Power, is capable of the Graphene particle tight on stalk powder surface after drying.Final in stalk powder particle surface shape
Becoming the protection layer of charcoal of a kind of densification, this layer of charcoal can completely cut off heat, gas so that the fuel gas that thermal decomposition produces is no longer participate in
Burning, the final raising fire-retardant performance of composite.
Detailed description of the invention
Illustrate below and the present invention is described in more detail
Embodiment 1:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 3 hours
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:100(g/ml) ratio mix after ultrasonic disperse 10min；
4) described composite mechanical agitation at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C be dried 12
Hour, it is thus achieved that the stalk powder of graphene oxide coating.
Embodiment 2:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 3 hours
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:150(g/ml) ratio mix after ultrasonic disperse 20min；
4) described composite mechanical agitation at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C be dried 12
Hour, it is thus achieved that the stalk powder of graphene oxide coating.
Embodiment 3:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 3 hours
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:200(g/ml) ratio mix after ultrasonic disperse 30min；
4) described composite mechanical agitation at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C be dried 12
Hour, it is thus achieved that the stalk powder of graphene oxide coating.
Embodiment 4:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 3 hours
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:300(g/ml) ratio mix after ultrasonic disperse 25min；
4) described composite mechanical agitation at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C be dried 12
Hour, it is thus achieved that the stalk powder of graphene oxide coating.
Embodiment 5:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 3 hours
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:400(g/ml) ratio mix after ultrasonic disperse 20min；
4) described composite mechanical agitation at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C be dried 12
Hour, it is thus achieved that the stalk powder of graphene oxide coating.
Embodiment 6:
1) straw medulla part is removed, with stalk fibre part as main raw material(s), dried powder under the conditions of 100 DEG C
It is milled to granularity and obtains stalk powder less than 100 μm；
2) it is 0.2mg/ that graphene oxide is placed in deionized water ultrasonic disperse obtains dispersed concentration after 3 hours
The graphene oxide water solution of ml-1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5:500(g/ml) ratio mix after ultrasonic disperse 10min；
4) described composite mechanical agitation at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C be dried 12
Hour, it is thus achieved that the stalk powder of graphene oxide coating.
Tested by following fire retardant performance and show the positive effect of the present invention:
Test method: dusty material prepared by above example 1-6 is prepared by die press technology for forming and met GB/
The sample that T2406.2-2009 requires, and it is as shown in the table to carry out its data of oxygen index (OI) performance test.
Experiment material: the stalk powder of the graphene oxide coating of embodiment 1 ~ embodiment 6 preparation.
Experimental result is shown in Table 1；
Subordinate list oxygen index (OI) related data
| Sequence number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Oxygen index (OI) (%) | 28.8 | 30.5 | 32.2 | 35.1 | 37.2 | 39.5 |
Conclusion: above-mentioned test shows that the fire retardant performance of product of the present invention is excellent, and anti-flammability reaches B1 level requirement.With
Time, have that preparation technology is simple, environmental protection, the advantage of nonhazardous.Achieve what stalk material utilized in building material field
High added value, and expand its range of application in Building Fire Protection fire proofing field.
Claims (1)
1. a graphene oxide fire-retardant stalk material preparation method, comprises the following steps:
1) straw medulla part being removed, with stalk fibre part as main raw material(s), under the conditions of 100 DEG C, dried grinding is extremely
Granularity obtains stalk powder less than 100 μm；
2) graphene oxide is placed in ultrasonic disperse in deionized water obtain after 2-4 hour dispersed concentration be 0.2mg/ml ~
The graphene oxide water solution of 1.5mg/ml；
3) by powder of straw with graphene oxide water solution in 5g:(100 ml ~ 500 ml) ratio mix after ultrasonic disperse 10-
30min；
4) described composite mechanical agitation at 80-90 DEG C is evaporated to mixture be thick after, at 50-60 DEG C be dried
12 hours, it is thus achieved that the stalk powder of graphene oxide coating.
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| CN201510428513.7A CN104986982B (en) | 2015-07-21 | 2015-07-21 | A kind of fire-retardant stalk material of graphene oxide and preparation method thereof |
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| CN201510428513.7A CN104986982B (en) | 2015-07-21 | 2015-07-21 | A kind of fire-retardant stalk material of graphene oxide and preparation method thereof |
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| CN104986982A CN104986982A (en) | 2015-10-21 |
| CN104986982B true CN104986982B (en) | 2016-08-31 |
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Families Citing this family (5)
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| CN109572099A (en) * | 2017-09-29 | 2019-04-05 | 中科众创（重庆）秸秆产业研究院有限公司 | A kind of composite plate and preparation method thereof containing crop straw |
| CN109575623A (en) * | 2017-09-29 | 2019-04-05 | 中科众创（重庆）秸秆产业研究院有限公司 | Stalk fire proofing and preparation method thereof based on dissaving polymer modified graphene |
| CN109575622A (en) * | 2017-09-29 | 2019-04-05 | 中科众创（重庆）秸秆产业研究院有限公司 | A kind of fire-retardant stalk compound material and preparation method thereof |
| CN112625342B (en) * | 2020-12-08 | 2022-12-13 | 广东聚石科技研究有限公司 | Graphene modified plastic and preparation method and application thereof |
| CN115558076B (en) * | 2022-09-08 | 2024-03-26 | 吉林大学 | Castor oil polyurethane material containing graphene oxide modified fibers and preparation method thereof |
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