CN105237816A - Preparation method and application of graphene oxide/sodium alginate liquid crystal composite solution - Google Patents
Preparation method and application of graphene oxide/sodium alginate liquid crystal composite solution Download PDFInfo
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- CN105237816A CN105237816A CN201510648291.XA CN201510648291A CN105237816A CN 105237816 A CN105237816 A CN 105237816A CN 201510648291 A CN201510648291 A CN 201510648291A CN 105237816 A CN105237816 A CN 105237816A
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Abstract
The invention discloses a preparation method of a graphene oxide/sodium alginate liquid crystal composite solution, wherein the preparation method includes the following steps: firstly, adding graphene oxide in deionized water to obtain a graphene oxide solution, wherein the concentration of the graphene oxide solution is 1-10 mg/mL; and then adding sodium alginate into the graphene oxide solution, to obtain a graphene oxide/sodium alginate liquid crystal composite solution, wherein the mass ratio of graphene oxide to sodium alginate in the graphene oxide/sodium alginate liquid crystal composite solution is 0.5-0.05. With the addition of sodium alginate (SA) in the graphene oxide (GO) solution, the formation of a liquid crystal phase is promoted; the prepared graphene oxide/sodium alginate liquid crystal composite solution has lower liquid crystal critical concentration, the preparation method is simple in process, easy to operate, low in cost and friendly to environment, and the product is easy to obtain. The preparation method is expected to prepare highly-oriented fiber and thin film materials and the like in lower graphene oxide (GO) concentration, and is more conducive to application of graphene oxide liquid crystals.
Description
Technical field
The present invention relates to method and the application of the formation of a kind of accelerating oxidation Graphene (GO) mesomorphic phase, specifically relate to preparation method and the application of a kind of graphene oxide/sodium alginate liquid crystal composite solution, belong to graphene oxide (GO) liquid crystal preparing technical field.
Background technology
The two-dirnentional structure that Graphene is intensive by one deck, the carbon atom arrangement be wrapped in honeycomb crystal lattice becomes, the existence of carbon six-ring stable in the two-dimension periodic honeycomb lattice structure of its uniqueness and structural unit, give the mechanical property of its excellence, thermal characteristics, optical property and electric property, be described as the hardest, conductivity best material in the world, add the energy-storage property of its excellence and large specific surface area, Graphene range of application is very wide.Graphene oxide (GO), as the important derivatives of Graphene, is generally obtained by chemical oxidation graphite.
In recent years, relevant graphene oxide (GO) liquid crystal and application thereof, receive much concern.Such as: GO liquid crystal can realize opto-electronic conversion by electric field induce sequence, also high strength fibre can be drawn out by wet-spinning, prepare anisotropy nano material as masterplate, therefore, to the preparation of graphene oxide (GO) mesomorphic phase and Research Significance great.The Critical concentration of GO has much relations with its length-to-diameter ratio, the acquisition of current GO mesomorphic phase, mainly by improving the length-to-diameter ratio of GO, realizes the mesomorphic phase obtaining GO in lower concentration, but its complicated process of preparation, cost is high, requires high to the length-to-diameter ratio of sample.
Summary of the invention
The object of the present invention is to provide preparation method and the application of a kind of graphene oxide/sodium alginate liquid crystal composite solution, the method by adding the formation that sodium alginate (SA) promotes its mesomorphic phase in graphene oxide (GO) solution, and obtained graphene oxide/sodium alginate liquid crystal composite solution has lower Critical concentration.
The technology used in the present invention solution is:
A preparation method for graphene oxide/sodium alginate liquid crystal composite solution, comprises the following steps:
(1) graphene oxide is added in deionized water, obtained graphene oxide solution;
(2) in the obtained graphene oxide solution of step (1), sodium alginate is added, obtained graphene oxide/sodium alginate liquid crystal composite solution.
Further, in step (1), the concentration of described graphene oxide solution is 1-10mg/mL.
Further, in step (1), comprise following concrete steps: be first scattered in deionized water by graphene oxide and carry out centrifuge washing, collect the slurry of thickness bottom centrifuge tube, lyophilize, in the slurry after lyophilize, add deionized water dilution again, obtain graphene oxide solution.During centrifuge washing, rotating speed is 9000r/min, and washing time is 30min.
Further, in step (1), described graphene oxide is that raw material adopts the correction Hummers method comprising two-step oxidation to prepare with natural graphite, specific as follows: in the preoxidation stage, first by 8.4gK
2s
2o
8and 8.4gP
2o
5be dispersed in the dense H of 40mL
2sO
4in, slowly add 10g natural graphite powder subsequently, at 80 DEG C, react 4.5h; After cool to room temperature, dilute with deionized water and place and spend the night; Be the cellulose mixture filter membrane suction filtration of 0.22 μm subsequently with aperture, and use 1.5L deionized water wash, in ice-water bath, products therefrom is poured into the dense H of 230mL
2sO
4in and ceaselessly stir, until temperature is down to 0-3 DEG C; Slowly 60gKMnO is added under stirring
4, and maintain the temperature at less than 10 DEG C, obtain mixed solution; Subsequently mixed solution is heated to 35 DEG C and stirs 2h, stir 30min again with after 0.5L deionized water wash; Add 1.5L deionized water and 25mL, 30% H
2o
2termination reaction; Leave standstill two days, discard supernatant liquor; Bottom settlings is filtered, and removes remaining metal ions with 1MHCl solution washing; Product is constantly used deionized water wash, and centrifugation, until washing lotion pH value reaches 6; Through lyophilize two days later, GO sample is obtained.
Sodium alginate (SA) is the linear natural polysaccharide material of one extracted from brown alga or bacterium, and its molecular weight ranges is at 50kDa-500kDa, and the lower promoter action to liquid crystal of molecular weight is stronger.
Further, in step (2), in described graphene oxide/sodium alginate liquid crystal composite solution, the mass ratio of graphene oxide and sodium alginate is 0.5-0.05.And the less promoter action to liquid crystal of its ratio is stronger.
Further, in step (2), in described graphene oxide/sodium alginate liquid crystal composite solution, the concentration of sodium alginate is 0.5mg/mL-150mg/mL, and the concentration of graphene oxide is 0.05mg/mL-25mg/mL.
Further, in step (2), described sodium alginate adds in graphene oxide solution in two steps, to ensure the homogeneity of sodium alginate soln, specific as follows: first small part sodium alginate to be added in graphene oxide solution, in the water-bath of 20-70 DEG C, stir 30min-45min, then ultrasonic through 30min-45min, again residue sodium alginate is added, stirring at room temperature 2-8h.Or first small part sodium alginate is added in graphene oxide solution, stirring at room temperature 2-8h, and then remaining sodium alginate is added, and 30min is stirred in the water-bath of 20-70 DEG C.
Further, in step (2), described graphene oxide/sodium alginate liquid crystal composite solution is observed under orthogonal polarizing microscope, has obvious liquid crystal feature, and liquid crystal is nematic or cholesteric.The threshold concentration of graphene oxide/sodium alginate liquid crystal composite solution can utilize rotational rheometer and polarizing microscope to measure.
Above-mentioned graphene oxide/sodium alginate liquid crystal composite solution can be applicable in the various fields such as fibrous woven, pharmaceutical preparation, food-processing, organizational project side.
Above-mentioned graphene oxide/sodium alginate liquid crystal composite solution can be applicable to aspects such as preparing anisotropic film, gel, fiber.
Advantageous Effects of the present invention is:
The present invention by adding the formation that sodium alginate (SA) promotes its mesomorphic phase in graphene oxide (GO) solution, the Critical concentration of obtained graphene oxide/sodium alginate liquid crystal composite solution drops to 0.1mg/mL, obvious reduction has been had, Be very effective compared with the Critical concentration 2mg/mL of graphene oxide sample.The present invention not only significantly can reduce the critical liquid crystal concentration of GO, and technique is very simple, easy to operate, with low cost, environmentally friendly, and product is easy to obtain.The present invention is expected to realize preparing height-oriented fiber and thin-film material etc. under the concentration of lower graphene oxide (GO), is more conducive to the application of Graphene liquid crystal.
Accompanying drawing explanation
The polarizing microscope figure of Fig. 1 to be concentration the be graphene oxide (GO) of 0.25mg/mL and sodium alginate (SA) liquid crystal composite solution of 80mg/mL; As can be seen from the figure composite solution has stronger anisotropy, and occurs the thread-like texture that row type liquid crystal has.
The polarizing microscope figure of Fig. 2 to be concentration the be graphene oxide (GO) of 1.25mg/mL and sodium alginate (SA) liquid crystal composite solution of 20mg/mL; As can be seen from the figure the anisotropic of composite solution obviously strengthens, and has the line layer texture that cholesteryl liquid crystal has.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
The preparation of graphene oxide (GO)
In the preoxidation stage, first by 8.4gK
2s
2o
8and 8.4gP
2o
5be dispersed in the dense H of 40mL
2sO
4in, slowly add 10g natural graphite powder subsequently, at 80 DEG C, react 4.5h.After cool to room temperature, dilute with deionized water and place and spend the night.Be the cellulose mixture filter membrane suction filtration of 0.22 μm subsequently with aperture, and use 1.5L deionized water wash.In ice-water bath, products therefrom is poured into the dense H of 230mL
2sO
4in and ceaselessly stir, until temperature is down to 0-3 DEG C.Slowly 60gKMnO is added under stirring
4, and maintain the temperature at less than 10 DEG C.Subsequently mixed solution is heated to 35 DEG C and stirs 2h, stir 30min again with after 0.5L deionized water wash.Add 1.5L deionized water and 25mL, 30% H
2o
2termination reaction.Leave standstill two days, discard supernatant liquor.Bottom settlings is filtered, and removes remaining metal ions with 1MHCl solution washing.Product is constantly used deionized water wash, and centrifugation, until washing lotion pH value reaches 6.Through lyophilize two days later, GO sample is obtained.
Get graphene oxide (GO) obtained in above-mentioned steps, add deionized water and be diluted to 1mg/mL, obtain GO solution.Get the GO solution of the 1mg/mL of 100mL, add the sodium alginate (SA) that 0.1g molecular weight is 300kDa and stir 30min, then make it homogenizing through 30min is ultrasonic; The SA adding 0.9g again continues to stir 2h, can obtain stable GO/SA liquid crystal composite solution.
Embodiment 2
The preparation of graphene oxide is with embodiment 1.
Get graphene oxide (GO), add deionized water and be diluted to 5mg/mL.Get the GO solution of the 5mg/mL of 100mL, adding 0.1g molecular weight is that 300kDa sodium alginate (SA) stirs 30min, then makes it homogenizing through 30min is ultrasonic; The SA adding 0.4g again continues to stir 2h, can obtain stable GO/SA liquid crystal composite solution.
Embodiment 3
The preparation of graphene oxide is with embodiment 1.
Graphene oxide (GO) in Example 1, adds deionized water and is diluted to 10mg/mL.Get the GO solution of the 10mg/mL of 100mL, adding 0.5g molecular weight is that 500kDa sodium alginate (SA) stirs 30min, then makes it homogenizing through 30min is ultrasonic; The SA adding 2.5g again continues to stir 2h, can obtain stable GO/SA liquid crystal composite solution.
Embodiment 4
Graphene oxide adopts conventional steps to obtain.
Get graphene oxide (GO), add deionized water and be diluted to 10mg/mL, obtained graphene oxide solution.Get the GO solution that 100mL concentration is 10mg/mL, adding 0.5g molecular weight is that 50kDa sodium alginate (SA) stirs 30min in the water-bath of 70 DEG C, then makes it homogenizing through 30min is ultrasonic; Add the SA continuation stirring 2h that 2.5g molecular weight is 50kDa again, stable GO/SA liquid crystal composite solution can be obtained.
Embodiment 5
The preparation of graphene oxide is with embodiment 1.
Get graphene oxide (GO), add deionized water and be diluted to 8mg/mL, obtained graphene oxide solution.Get the GO solution that 100mL concentration is 8mg/mL, adding 0.5g molecular weight is that 100kDa sodium alginate (SA) stirs 30min in the water-bath of 50 DEG C, then makes it homogenizing through 30min is ultrasonic; Add the SA continuation stirring 2h that 5.5g molecular weight is 100kDa again, stable GO/SA liquid crystal composite solution can be obtained.
GO/SA liquid crystal composite solution obtained in above-described embodiment can prepare anisotropic films, gel, fiber, can be applied in the various fields such as fibrous woven, pharmaceutical preparation, food-processing, organizational project.
Claims (10)
1. a preparation method for graphene oxide/sodium alginate liquid crystal composite solution, is characterized in that comprising the following steps:
(1) graphene oxide is added in deionized water, obtained graphene oxide solution;
(2) in the obtained graphene oxide solution of step (1), sodium alginate is added, obtained graphene oxide/sodium alginate liquid crystal composite solution.
2. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, is characterized in that, in step (1), the concentration of described graphene oxide solution is 1-10mg/mL.
3. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, it is characterized in that, in step (1), comprise following concrete steps: be first scattered in deionized water by graphene oxide and carry out centrifuge washing, collect the slurry of thickness bottom centrifuge tube, lyophilize, then in the slurry after lyophilize, add deionized water dilution, obtain graphene oxide solution.
4. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, it is characterized in that, in step (1), described graphene oxide is that raw material adopts the correction Hummers method comprising two-step oxidation to prepare with natural graphite, specific as follows: in the preoxidation stage, first by 8.4gK
2s
2o
8and 8.4gP
2o
5be dispersed in the dense H of 40mL
2sO
4in, slowly add 10g natural graphite powder subsequently, at 80 DEG C, react 4.5h; After cool to room temperature, dilute with deionized water and place and spend the night; Be the cellulose mixture filter membrane suction filtration of 0.22 μm subsequently with aperture, and use 1.5L deionized water wash, in ice-water bath, products therefrom is poured into the dense H of 230mL
2sO
4in and ceaselessly stir, until temperature is down to 0-3 DEG C; Slowly 60gKMnO is added under stirring
4, and maintain the temperature at less than 10 DEG C, obtain mixed solution; Subsequently mixed solution is heated to 35 DEG C and stirs 2h, stir 30min again with after 0.5L deionized water wash; Add 1.5L deionized water and 25mL, 30% H
2o
2termination reaction; Leave standstill two days, discard supernatant liquor; Bottom settlings is filtered, and removes remaining metal ions with 1MHCl solution washing; Product is constantly used deionized water wash, and centrifugation, until washing lotion pH value reaches 6; Through lyophilize two days later, GO sample is obtained.
5. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, it is characterized in that, in step (2), in described graphene oxide/sodium alginate liquid crystal composite solution, the mass ratio of graphene oxide and sodium alginate is 0.5-0.05.
6. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, it is characterized in that, in step (2), in described graphene oxide/sodium alginate liquid crystal composite solution, the concentration of sodium alginate is 0.5mg/mL-150mg/mL, and the concentration of graphene oxide is 0.05mg/mL-25mg/mL.
7. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, it is characterized in that, in step (2), described sodium alginate adds in graphene oxide solution in two steps, specific as follows: first small part sodium alginate to be added in graphene oxide solution, in the water-bath of 20-70 DEG C, stir 30min-45min, then ultrasonic through 30min-45min, again residue sodium alginate is added, stirring at room temperature 2-8h.
8. the preparation method of a kind of graphene oxide according to claim 1/sodium alginate liquid crystal composite solution, it is characterized in that, in step (2), described graphene oxide/sodium alginate liquid crystal composite solution is observed under orthogonal polarizing microscope, have obvious liquid crystal feature, liquid crystal is nematic or cholesteric.
9. the graphene oxide as described in claim arbitrary in the claim 1-8/application of sodium alginate liquid crystal composite solution in fibrous woven, pharmaceutical preparation, food-processing, organizational project.
10. the graphene oxide as described in claim arbitrary in claim 1-8/sodium alginate liquid crystal composite solution is preparing the application in anisotropic film, gel, fiber.
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| CN111424337A (en) * | 2020-04-07 | 2020-07-17 | 东华大学 | Method for preparing chiral reversal graphene liquid crystal through nano fluid rectification |
| CN112267174A (en) * | 2020-10-26 | 2021-01-26 | 江南大学 | Method for preparing electrochromic fiber without external electrode by coaxial microfluid spinning method |
| CN112937013A (en) * | 2021-01-28 | 2021-06-11 | 上海大学 | High-thermal-conductivity and three-level shape memory multilayer structure flexible film and preparation method thereof |
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| CN105833851A (en) * | 2016-05-18 | 2016-08-10 | 同济大学 | Method for preparing functional group modified alginate-graphene dual-network nano-composite gel beads |
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| CN110195271B (en) * | 2019-06-27 | 2021-11-12 | 中素新科技有限公司 | Graphene aerogel fibers, and preparation method and application thereof |
| CN111424337A (en) * | 2020-04-07 | 2020-07-17 | 东华大学 | Method for preparing chiral reversal graphene liquid crystal through nano fluid rectification |
| CN112267174A (en) * | 2020-10-26 | 2021-01-26 | 江南大学 | Method for preparing electrochromic fiber without external electrode by coaxial microfluid spinning method |
| CN112267174B (en) * | 2020-10-26 | 2021-11-02 | 江南大学 | Method for preparing electrochromic fiber without external electrode by coaxial microfluid spinning method |
| CN112937013A (en) * | 2021-01-28 | 2021-06-11 | 上海大学 | High-thermal-conductivity and three-level shape memory multilayer structure flexible film and preparation method thereof |
| CN113184832A (en) * | 2021-03-09 | 2021-07-30 | 中国科学院兰州化学物理研究所 | Flexible three-dimensional graphene aerogel, preparation method and application thereof, flexible three-dimensional graphene-based piezoresistive sensor and application thereof |
| CN114887498A (en) * | 2022-06-21 | 2022-08-12 | 青岛大学 | Graphene oxide/sodium alginate composite nanofiltration membrane with controllable water flux or rejection rate |
| CN114887498B (en) * | 2022-06-21 | 2023-09-22 | 青岛大学 | Graphene oxide/sodium alginate composite nanofiltration membrane with controllable water flux or retention rate |
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