CN104986982A - Graphene oxide flame-retardant straw material and preparation method therefor - Google Patents
Graphene oxide flame-retardant straw material and preparation method therefor Download PDFInfo
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- CN104986982A CN104986982A CN201510428513.7A CN201510428513A CN104986982A CN 104986982 A CN104986982 A CN 104986982A CN 201510428513 A CN201510428513 A CN 201510428513A CN 104986982 A CN104986982 A CN 104986982A
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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 invention provides a graphene oxide flame-retardant straw material and a preparation method therefor. After drying straw fiber, mechanically grinding the straw fiber till the granularity is less than 100 [mu]m; putting graphene oxide in deionized water and carrying out ultrasonic dispersion for 3 hours to obtain a uniform graphene oxide aqueous solution with dispersion concentration of 0.2-1 mg/ml; pouring mechanically ground straw powder into the graphene oxide aqueous solution and carrying out ultrasonic dispersion for 30 minutes; and stirring and evaporating the dispersed mixed system at 90 DEG C till the system is thick and drying the system at 60 DEG C to remove residual water so as to obtain the graphene oxide flame-retardant straw material coated with one or more layers of graphene oxide. The graphene oxide flame-retardant straw material is simple in preparation process and environmental-friendly, provides a novel path for developing application of straws in the field of building materials, and has a broad application prospect.
Description
technical field:
What the present invention relates to is fire-retardant stalk material of a kind of graphene oxide and preparation method thereof, belongs to fire protection flame retarding building material technical field.
background technology:
China is a large agricultural country, and stalk resource is very abundant, and distribution is wide, kind is many and output 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 30% of whole world stalk total amount.According to investigations, current China straw utilization rate is about 33%, and major part does not add process, and what utilize after technical finesse only accounts for about 2.6%.Stalk is main based on building block, sheet material in building material field application.But in application process, there is the problems such as goods are inflammable, corrosion-resistant, added value are not high.Therefore, exploitation stalk novelty teabag, improves stalk self performance, promotes its added value, improve it and have practical significance in the application of field of functional materials.
Graphene is owing to having high-specific surface area, and excellent thermostability, electric property and mechanical property, be subject to extensive concern in the research in the fields such as matrix material enhancing and conduction.In graphene nano material preparation process, the Van der Waals force of graphene film interlayer is often considered to the subject matter hindering graphene dispersion.If in building material field, we utilize the thermostability of Graphene excellence and the Van der Waals force of graphene film interlayer, under the condition not adding other properties-correcting agent, preparation has the graphene oxide stalk compound material of core-shell structure, under reaching the state using less filler, and significantly promoting the fire retardant performance of matrix material, this will promote the development and progression of Novel fireproof flame-retardant material.Compare ubiquity preparation technology relative complex in traditional building material flame retardant area, fire retardant burning bring the problem of smoke toxicity, the present invention to have preparation technology is simple, environmental protection, toxicological harmless advantage.This research there is no report at home and abroad.
summary of the invention:
The object of this invention is to provide the fire-retardant stalk material of a kind of graphene oxide and preparation method, technique be simple, with low cost, environmental friendliness, inflammable stalk can be made to become the material preparation method with flame retardant properties.
the fire-retardant stalk material preparation method of a kind of graphene oxide of the present invention, comprises the following steps:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in deionized water for ultrasonic dispersion and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml after 2-4 hour;
3) by straw powder with graphene oxide water solution in 5:(100 ~ 500) ratio of (g/ml) mix after ultrasonic disperse 10-30min;
4) described matrix material mechanical stirring at 80-90 DEG C is evaporated to mixture be thick after, at 50-60 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
Described stalk is one or more mixtures in maize straw, wheat stalk, rice straw, broomcorn straw.
The flame retardant properties of product of the present invention can reach B1 level.
positively effect of the present invention is:take graphene oxide as properties-correcting agent, under spin coating evaporation technology, realize the coating of graphene oxide at stalk powder particle surface, thus the obtained fire-retardant stalk material of graphene oxide.Theoretical foundation of the present invention is: because Graphene has high-specific surface area, excellent thermostability, stronger Van der Waals force, along with in solution evaporation process, the concentration of graphene oxide constantly promotes, along with high-speed stirring, under physics chemical action with stalk powder particle for reactive center, realize the attachment of graphene oxide at stalk particle surface.And because graphene film interlayer has stronger Van der Waals force, the tight parcel of Graphene particle on stalk powder surface after drying, can be realized.The final protection layer of charcoal forming a kind of densification at stalk powder particle surface, this layer of charcoal can completely cut off heat, gas, and the inflammable gas that thermolysis is produced no longer participates in burning, the fire-retardant performance of final raising matrix material.
Embodiment
Illustrate below and the present invention is described in more detail
embodiment 1:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in after deionized water for ultrasonic disperses 3 hours and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml;
3) by straw powder with graphene oxide water solution in 5:100(g/ml) ratio mix after ultrasonic disperse 10min;
4) described matrix material mechanical stirring at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
embodiment 2:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in after deionized water for ultrasonic disperses 3 hours and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml;
3) by straw powder with graphene oxide water solution in 5:150(g/ml) ratio mix after ultrasonic disperse 20min;
4) described matrix material mechanical stirring at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
embodiment 3:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in after deionized water for ultrasonic disperses 3 hours and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml;
3) by straw powder with graphene oxide water solution in 5:200(g/ml) ratio mix after ultrasonic disperse 30min;
4) described matrix material mechanical stirring at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
embodiment 4:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in after deionized water for ultrasonic disperses 3 hours and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml;
3) by straw powder with graphene oxide water solution in 5:300(g/ml) ratio mix after ultrasonic disperse 25min;
4) described matrix material mechanical stirring at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
embodiment 5:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in after deionized water for ultrasonic disperses 3 hours and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml;
3) by straw powder with graphene oxide water solution in 5:400(g/ml) ratio mix after ultrasonic disperse 20min;
4) described matrix material mechanical stirring at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
embodiment 6:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in after deionized water for ultrasonic disperses 3 hours and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml;
3) by straw powder with graphene oxide water solution in 5:500(g/ml) ratio mix after ultrasonic disperse 10min;
4) described matrix material mechanical stirring at 90 DEG C is evaporated to mixture be thick after, at 55 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
positively effect of the present invention is shown by following fire retardant performance test:
test method:the sample meeting GB/T2406.2-2009 and require prepared by powdered material prepared by above embodiment 1-6 by die press technology for forming, and it is as shown in the table to carry out its data of oxygen index performance test.
experiment material:the stalk powder of graphene oxide coating prepared by embodiment 1 ~ embodiment 6.
Experimental result is in table 1;
Subordinate list oxygen index related data
| Sequence number | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Oxygen index (%) | 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 flame retardant resistance reaches the requirement of B1 level.Meanwhile, have that preparation technology is simple, environmental protection, toxicological harmless advantage.Achieve the high added value that stalk material utilizes in building material field, and expand its range of application in Building Fire Protection fire retardant material field.
Claims (2)
1. the fire-retardant stalk material preparation method of graphene oxide, comprises the following steps:
1) by stalk medulla partial removal, with stalk fibre part for main raw material(s), after dry under 100 DEG C of conditions, grinding to granularity is less than 100 μm and obtains stalk powder;
2) graphene oxide is placed in deionized water for ultrasonic dispersion and obtains the graphene oxide water solution that dispersed concentration is 0.2mg/ml-1.5mg/ml after 2-4 hour;
3) by straw powder with graphene oxide water solution in 5:(100 ~ 500) ratio of (g/ml) mix after ultrasonic disperse 10-30min;
4) described matrix material mechanical stirring at 80-90 DEG C is evaporated to mixture be thick after, at 50-60 DEG C dry 12 hours, obtain the stalk powder of graphene oxide coating.
2. the preparation method of graphene oxide straw fireproof fire retardant material according to claim 1, is characterized in that: described stalk is one or more mixtures in maize straw, wheat stalk, rice straw, broomcorn straw.
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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 true CN104986982A (en) | 2015-10-21 |
| CN104986982B CN104986982B (en) | 2016-08-31 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112625342A (en) * | 2020-12-08 | 2021-04-09 | 广东聚石科技研究有限公司 | Graphene modified plastic and preparation method and application thereof |
| CN115558076A (en) * | 2022-09-08 | 2023-01-03 | 吉林大学 | Castor oil polyurethane material containing graphene oxide modified fibers and preparation method thereof |
-
2015
- 2015-07-21 CN CN201510428513.7A patent/CN104986982B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112625342A (en) * | 2020-12-08 | 2021-04-09 | 广东聚石科技研究有限公司 | Graphene modified plastic and preparation method and application thereof |
| CN115558076A (en) * | 2022-09-08 | 2023-01-03 | 吉林大学 | Castor oil polyurethane material containing graphene oxide modified fibers and preparation method 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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| CN104986982B (en) | 2016-08-31 |
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