CN105731933A - Preparation method of graphene oxide/high-strength concrete composite material - Google Patents
Preparation method of graphene oxide/high-strength concrete composite material Download PDFInfo
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- CN105731933A CN105731933A CN201610114477.1A CN201610114477A CN105731933A CN 105731933 A CN105731933 A CN 105731933A CN 201610114477 A CN201610114477 A CN 201610114477A CN 105731933 A CN105731933 A CN 105731933A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical Kinetics & Catalysis (AREA)
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the technical field of composite material preparation, and relates to a preparation method of a graphene oxide/high-strength concrete composite material. The preparation method specifically comprises the following steps: (1) preparing preoxidized graphite powder through a pretreatment process; (2) after mixing the preoxidized graphite powder with concentrated sulfuric acid and potassium permanganate, and then diluting by distilled water, oxidizing by an aqueous hydrogen peroxide solution, and carrying out acid washing by an aqueous hydrochloric acid solution; (3) stirring and blending the solution subjected to the acid washing by an aqueous sodium hydroxide solution and then performing freeze drying to prepare graphene oxide powder; (4) compounding the following components in parts by weight respectively: 0.5 to 1.2 parts of water, 4 parts of cement, 0.5 to 3.5 parts of silica fume, 5 to 8 parts of fine aggregates, 7 to 15 parts of coarse aggregates, 0.02 to 0.6 part of a water reducer and 0.001 to 0.1 part of graphene oxide powder, thus obtaining the graphene oxide/high-strength concrete composite material. The method disclosed by the invention is scientific in design, reliable in principles, convenient to operate, simple in process and strong in controllability, thereby being suitable for large-scale industrial production.
Description
Technical field:
The invention belongs to technical field of composite preparation, the preparation method relating to a kind of graphene oxide/high-strength concrete composite, prepared graphene oxide/high-strength concrete composite has good comprcssive strength.
Background technology:
Development and scientific and technological progress along with society, the construction of the every infrastructure of China is also gradually improved, along with the continuous construction of numerous urban subject facilities such as transportation, airport, harbour, bridge, communication, water conservancy and city water supply and sewage, concrete consumption and quality are also more and more most important.The prescription that various facilities are improved constantly also is the challenge of the performance indications to structural material, although present stage, various new material continued to bring out, but xoncrete structure is still seized of absolute status in every infrastructure construction, therefore getting more and more with concrete service condition under extensive, extreme environmental conditions, concrete property indices is in the urgent need to being further improved.
Graphene oxide (grapheneoxide) is the oxide of Graphene, and its color is brown color, and product common on the market has Powdered, lamellar and solution shape；Because of after oxidized on it oxygen-containing functional group increase and make its character relatively Graphene more active.Graphene oxide thin slice is powdered graphite through chemical oxidation and the product after peeling off, graphene oxide is single atomic layer, it is possible to expand to some tens of pm at any time on lateral dimension, therefore, and its construct trans typical size of general chemistry and material science.Graphene oxide can be considered the flexible material of a kind of non-traditional kenel, has polymer, colloid, thin film and amphiphilic characteristic, also has amphipathic simultaneously, and it presents hydrophilic to hydrophobic property distribution from edge to central authorities；Therefore, if graphene oxide is incorporated in concrete, the formation of hydrated cementitious crystal can be played template action by stannic oxide/graphene nano lamella, thus cement being improved in microstructure, to change shape and the arrangement mode of aquation crystal, thus playing the effect improving concrete comprcssive strength；And currently available technology yet there are no technique or the method for preparing concrete and composite thereof with graphene oxide；So, the preparation method that the present invention designs a kind of graphene oxide/high-strength concrete composite, by mixing match such as prepared graphene oxide powder and water, water reducer, silicon ash, medium sand, granite stones, make the graphene oxide/high-strength concrete composite of a kind of high intensity, there is good application prospect.
Summary of the invention:
The goal of the invention of the present invention is in that the shortcoming overcoming prior art to exist, seek the preparation method designing a kind of graphene oxide/high-strength concrete composite, it is mixed in high-strength concrete by prepared graphene oxide powder mixture ratio, to prepare the graphene oxide/high-strength concrete composite with good comprcssive strength.
To achieve these goals, the preparation method of the graphene oxide that the present invention relates to/high-strength concrete composite specifically includes following processing step:
(1) preprocessing process: take concentrated sulphuric acid, 8g potassium peroxydisulfate and 8g phosphorus pentoxide mix homogeneously that 55ml mass fraction is 98% and heat to 80 DEG C until being completely dissolved formation mixed liquor；Take 16g graphite powder to add under the mixing speed of 400～500r/min in mixed liquor, and make graphite powder and mixed liquor aoxidize at 20～25 DEG C of room temperature with constant stirring 6h, oxidation is rinsed to pH=7 with 500ml distilled water diluting mixture sucking filtration after terminating, then 4 hours prepared pre-oxidation powdered graphites of vacuum drying under 35～45 DEG C of conditions；
(2) oxidizing process: take the pre-oxidation powdered graphite prepared in step (1) and mix under 0 DEG C of condition of ice bath with the concentrated sulphuric acid of 450ml mass fraction 98%, temperature 0 DEG C, it is slow added into 48g potassium permanganate powder after stirring 10～20min and 10 DEG C of continuously stirred 10～20min of temperature control make mixture, then mixture is placed in 35 DEG C of stirred in water bath reaction 2h, being slow added into 500～700ml distilled water and keep reaction 20min at 90～100 DEG C of temperature, reaction adds 2200ml distilled water after terminating and is diluted；Add aqueous hydrogen peroxide solution to the mixture solution that 40ml molar concentration is 30% after dilution while stirring and all become golden yellow, be eventually adding the aqueous hydrochloric acid solution that 2200ml mass fraction is 2-3% and carry out pickling, then the centrifugal 10min when 3000r/min；Repeat above-mentioned pickling twice；
(3) last handling process: add 2～3L distilled water in step (2) in solution after pickling centrifugal once, being stirred being in harmonious proportion, with the sodium hydrate aqueous solution that pH is 10～11, the pH value making solution after outwelling the supernatant is 7, and solution is finally dried to graphene oxide powder in freezer dryer；
(4) concrete composite material preparation: weigh according to weight ratio respectively 0.5～1.2 part of water, cement 4 parts, silicon ash 0.5～3.5 part, fine aggregate 5～8 parts, coarse aggregate 7～15 parts, water reducer 0.02～0.6 part, 0.001～0.1 part of graphene oxide powder, load weighted graphene oxide powder is mixed with water and water reducer, to be mixed uniformly after mix with cement, silicon ash, fine aggregate and coarse aggregate again, stirring is to prepared graphene oxide/high-strength concrete composite after uniformly.
Further, cement is Portland cement, the intensity portland cement be more than or equal to 42.5 or Portland pozzolana cement；Fine aggregate is modulus of fineness is the medium sand of 2.0-4.0, and coarse aggregate is particle diameter is the continuous level granite stones between 10～30mm, diabase gravel and/or marble rubble；Water reducer is high-efficiency water-reducing agent of poly-carboxylic acid, and water is pH value is 47 ordinary tap water, and silicon ash can be selected for flyash, F breeze or slag and substitutes.
Compared with prior art, by by mixing match such as graphene oxide powder and fine aggregate, water, coarse aggregates, the graphene oxide made/high-strength concrete composite has good comprcssive strength to the present invention；The method design science, principle is reliable, easy and simple to handle, and process is simple, and controllability is strong, is suitable for large-scale industrial production.
Accompanying drawing illustrates:
Fig. 1 is the process flow diagram of the preparation method of the graphene oxide/high-strength concrete composite that the present invention relates to.
Detailed description of the invention:
Below in conjunction with accompanying drawing and by embodiment, the present invention is described in further detail, but the invention is not limited in implementation below.
Embodiment 1:
Concretely comprising the following steps of the preparation method of the graphene oxide related in the present embodiment/high-strength concrete composite:
(1) preprocessing process: take concentrated sulphuric acid, 8g potassium peroxydisulfate and 8g phosphorus pentoxide mix homogeneously that 55ml mass fraction is 98% and heat to 80 DEG C until being completely dissolved formation mixed liquor；Take 16g graphite powder to add under the mixing speed of 400～500r/min in mixed liquor, and make graphite powder and mixed liquor aoxidize at 20～25 DEG C of room temperature with constant stirring 6h, oxidation is rinsed to neutral (pH=7), then 4 hours prepared pre-oxidation powdered graphites of vacuum drying under 35～45 DEG C of conditions with 500ml distilled water diluting mixture sucking filtration after terminating；
(2) oxidizing process: take the pre-oxidation powdered graphite prepared in step (1) and mix under 0 DEG C of condition of ice bath with the concentrated sulphuric acid of 450ml mass fraction 98%, temperature 0 DEG C, it is slow added into 48g potassium permanganate powder after stirring 10～20min and 10 DEG C of continuously stirred 10～20min of temperature control make mixture, then mixture is placed in 35 DEG C of stirred in water bath reaction 2h, being slow added into 500～700ml distilled water and keep reaction 20min at 90～100 DEG C of temperature, reaction adds 2200ml distilled water after terminating and is diluted；Add aqueous hydrogen peroxide solution to the mixture solution that 40ml molar concentration is 30% after dilution while stirring and all become golden yellow, be eventually adding the aqueous hydrochloric acid solution that 2200ml mass fraction is 2-3% and carry out pickling, then the centrifugal 10min when 3000r/min；Repeat above-mentioned pickling twice；
(3) last handling process: add 2～3L distilled water in step (2) in solution after pickling centrifugal once, being stirred being in harmonious proportion, with the sodium hydrate aqueous solution that pH is 10～11, the pH value making solution after outwelling the supernatant is 7, finally by solution in freezer dryer dry to become graphene oxide powder；
(4) concrete composite material preparation: water, cement, silicon ash, medium sand, granite stones, water reducer, graphene oxide powder are weighed according to weight ratio 7:24:5.09:39.15:69.53:0.278:0.01-0.03, load weighted graphene oxide powder is mixed with water and water reducer, to be mixed uniformly after mix with cement, silicon ash, medium sand and granite stones again, stirring is to prepared graphene oxide/high-strength concrete composite after uniformly.
The cement related in the present embodiment is common 42.5 portland cements, and the modulus of fineness of medium sand is 2.0-4.0, and the particle diameter of granite stones is 10mm-30mm, and water reducer is high-efficiency water-reducing agent of poly-carboxylic acid, and water is pH value is the ordinary tap water of 47.
Prepared graphene oxide/high-strength concrete composite sampling is carried out intensity test by the present embodiment；Concrete Sample FormulationsThe (as shown in table 1) (wherein formula 6 is reference group):
| Formula number | Water | Cement | Silicon ash | Medium sand | Granite stones | Water reducer | Graphene oxide powder |
| 1 | 7 | 24 | 5.09 | 39.15 | 69.53 | 0.278 | 0.0144 |
| 2 | 7 | 24 | 5.09 | 39.15 | 69.53 | 0.278 | 0.0192 |
| 3 | 7 | 24 | 5.09 | 39.15 | 69.53 | 0.278 | 0.024 |
| 4 | 7 | 24 | 5.09 | 39.15 | 69.53 | 0.278 | 0.0288 |
| 5 | 7 | 24 | 5.09 | 39.15 | 69.53 | 0.278 | 0.0336 |
| 6 | 7 | 24 | 5.09 | 39.15 | 69.53 | 0.278 | 0 |
Sample FormulationsThe often organized by table 1
Each formula sample takes three groups of samplings test, each be sampled as the sample after maintenance 28 days；Testing standard is tested according to GB/T17671-1999 " Test method for strength of hydraulic cement mortar ", test result (as shown in table 2):
Table 2 intensity test (MPa)
As seen from the above table, the sample sampling comprcssive strength of formula 4 is best, compares and reference group 6 comprcssive strength improves 20.29%.
The foregoing is only the better embodiment of the present invention, protection scope of the present invention is not limited with above-mentioned embodiment, as long as the equivalence change that those skilled in the art make according to content of the present invention, all should include in protection scope of the present invention.
Claims (2)
1. the preparation method of graphene oxide/high-strength concrete composite, it is characterised in that specifically include following processing step:
(1) preprocessing process: take concentrated sulphuric acid, 8g potassium peroxydisulfate and 8g phosphorus pentoxide mix homogeneously that 55ml mass fraction is 98% and heat to 80 DEG C until being completely dissolved formation mixed liquor；Take 16g graphite powder to add under the mixing speed of 400～500r/min in mixed liquor, and make graphite powder and mixed liquor aoxidize at 20～25 DEG C of room temperature with constant stirring 6h, oxidation is rinsed to pH=7 with 500ml distilled water diluting mixture sucking filtration after terminating, then 4 hours prepared pre-oxidation powdered graphites of vacuum drying under 35～45 DEG C of conditions；
(2) oxidizing process: take the pre-oxidation powdered graphite prepared in step (1) and mix under 0 DEG C of condition of ice bath with the concentrated sulphuric acid of 450ml mass fraction 98%, temperature 0 DEG C, it is slow added into 48g potassium permanganate powder after stirring 10～20min and 10 DEG C of continuously stirred 10～20min of temperature control make mixture, then mixture is placed in 35 DEG C of stirred in water bath reaction 2h, being slow added into 500～700ml distilled water and keep reaction 20min at 90～100 DEG C of temperature, reaction adds 2200ml distilled water after terminating and is diluted；Add aqueous hydrogen peroxide solution to the mixture solution that 40ml molar concentration is 30% after dilution while stirring and all become golden yellow, be eventually adding the aqueous hydrochloric acid solution that 2200ml mass fraction is 2-3% and carry out pickling, then the centrifugal 10min when 3000r/min；Repeat above-mentioned pickling twice；
(3) last handling process: add 2～3L distilled water in step (2) in solution after pickling centrifugal once, being stirred being in harmonious proportion, with the sodium hydrate aqueous solution that pH is 10～11, the pH value making solution after outwelling the supernatant is 7, and solution is finally dried to graphene oxide powder in freezer dryer；
(4) concrete composite material preparation: weigh according to weight ratio respectively 0.5～1.2 part of water, cement 4 parts, silicon ash 0.5～3.5 part, fine aggregate 5～8 parts, coarse aggregate 7～15 parts, water reducer 0.02～0.6 part, 0.001～0.1 part of graphene oxide powder, load weighted graphene oxide powder is mixed with water and water reducer, to be mixed uniformly after mix with cement, silicon ash, fine aggregate and coarse aggregate again, stirring is to prepared graphene oxide/high-strength concrete composite after uniformly.
2. the preparation method of graphene oxide according to claim 1/high-strength concrete composite, it is characterised in that described cement is the intensity portland cement be more than or equal to 42.5 or Portland pozzolana cement；Fine aggregate is modulus of fineness is the medium sand of 2.0-4.0, and coarse aggregate is particle diameter is the continuous level granite stones of 10～30mm, diabase gravel and/or marble rubble；Water reducer is high-efficiency water-reducing agent of poly-carboxylic acid；Water is pH value is 47 ordinary tap water；Silicon ash can substitute with flyash or slag.
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Cited By (14)
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| CN106430174A (en) * | 2016-10-09 | 2017-02-22 | 黎明职业大学 | Monolithic graphene oxide aqueous dispersing solution and preparation method thereof |
| CN106431137A (en) * | 2016-09-21 | 2017-02-22 | 太原理工大学 | Grapheme concrete and preparation method thereof |
| CN106746834A (en) * | 2016-11-28 | 2017-05-31 | 中铁十二局集团有限公司 | A kind of graphene-based nanocrystal class early strength agent and preparation method thereof |
| CN107311569A (en) * | 2017-07-19 | 2017-11-03 | 太原理工大学 | Carboxyl-functional graphene oxide high performance concrete and preparation method thereof |
| CN107353397A (en) * | 2017-07-27 | 2017-11-17 | 江苏丰彩新型建材有限公司 | A kind of graphene water-base epoxy high dispersive system and its synthetic method |
| CN108117335A (en) * | 2017-12-19 | 2018-06-05 | 佛山科学技术学院 | A kind of graphene oxide concrete of fly ash and preparation method thereof |
| CN108147749A (en) * | 2018-01-15 | 2018-06-12 | 威海南海碳材料科技研究院有限公司 | A kind of graphene oxide foamed concrete and its preparation process |
| CN108314380A (en) * | 2018-01-31 | 2018-07-24 | 广州大学 | A kind of graphene oxide-ferroso-ferric oxide magnetic liquid-cement-base composite material and preparation method thereof |
| CN108424082A (en) * | 2018-04-19 | 2018-08-21 | 俞小峰 | A kind of preparation method of pleat-free cement-base waterproof coating |
| CN108547408A (en) * | 2018-04-23 | 2018-09-18 | 威海南海新能源材料有限公司 | A kind of graphene colored steel composite board insulation of fire resisting and preparation method thereof |
| CN110395951A (en) * | 2018-04-25 | 2019-11-01 | 陕西燕园众欣石墨烯科技有限公司 | A kind of graphene concrete composite material of chloride-penetration resistance and preparation method thereof |
| CN110407537A (en) * | 2019-07-31 | 2019-11-05 | 大连理工大学 | A kind of graphene reinforced reactive-powder-concrete of impact resistance |
| CN110606713A (en) * | 2019-09-20 | 2019-12-24 | 成都志达商品混凝土厂 | High-strength light aggregate concrete and preparation process thereof |
| CN111138150A (en) * | 2020-01-09 | 2020-05-12 | 新疆宏宇志祥工程咨询有限公司 | Preparation method of graphene oxide/carbon nanotube high-strength building concrete |
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| CN106430174A (en) * | 2016-10-09 | 2017-02-22 | 黎明职业大学 | Monolithic graphene oxide aqueous dispersing solution and preparation method thereof |
| CN106746834A (en) * | 2016-11-28 | 2017-05-31 | 中铁十二局集团有限公司 | A kind of graphene-based nanocrystal class early strength agent and preparation method thereof |
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| CN107311569A (en) * | 2017-07-19 | 2017-11-03 | 太原理工大学 | Carboxyl-functional graphene oxide high performance concrete and preparation method thereof |
| CN107353397B (en) * | 2017-07-27 | 2019-08-13 | 江苏丰彩新型建材有限公司 | A kind of preparation method of ultra high strength concrete |
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| CN108117335A (en) * | 2017-12-19 | 2018-06-05 | 佛山科学技术学院 | A kind of graphene oxide concrete of fly ash and preparation method thereof |
| CN108147749A (en) * | 2018-01-15 | 2018-06-12 | 威海南海碳材料科技研究院有限公司 | A kind of graphene oxide foamed concrete and its preparation process |
| CN108314380A (en) * | 2018-01-31 | 2018-07-24 | 广州大学 | A kind of graphene oxide-ferroso-ferric oxide magnetic liquid-cement-base composite material and preparation method thereof |
| CN108314380B (en) * | 2018-01-31 | 2020-11-13 | 广州大学 | Graphene oxide-ferroferric oxide magnetic liquid-cement-based composite material and preparation method thereof |
| CN108424082A (en) * | 2018-04-19 | 2018-08-21 | 俞小峰 | A kind of preparation method of pleat-free cement-base waterproof coating |
| CN108547408A (en) * | 2018-04-23 | 2018-09-18 | 威海南海新能源材料有限公司 | A kind of graphene colored steel composite board insulation of fire resisting and preparation method thereof |
| CN110395951A (en) * | 2018-04-25 | 2019-11-01 | 陕西燕园众欣石墨烯科技有限公司 | A kind of graphene concrete composite material of chloride-penetration resistance and preparation method thereof |
| CN110407537A (en) * | 2019-07-31 | 2019-11-05 | 大连理工大学 | A kind of graphene reinforced reactive-powder-concrete of impact resistance |
| CN110606713A (en) * | 2019-09-20 | 2019-12-24 | 成都志达商品混凝土厂 | High-strength light aggregate concrete and preparation process thereof |
| CN111138150A (en) * | 2020-01-09 | 2020-05-12 | 新疆宏宇志祥工程咨询有限公司 | Preparation method of graphene oxide/carbon nanotube high-strength building concrete |
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