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CN103768960B - A kind of preparation method of Graphene basement membrane and the application in water-oil separating thereof - Google Patents

A kind of preparation method of Graphene basement membrane and the application in water-oil separating thereof Download PDF

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CN103768960B
CN103768960B CN201410004581.6A CN201410004581A CN103768960B CN 103768960 B CN103768960 B CN 103768960B CN 201410004581 A CN201410004581 A CN 201410004581A CN 103768960 B CN103768960 B CN 103768960B
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graphene
oil
water
preparation
graphene oxide
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CN103768960A (en
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王兴
袁其朋
李国锋
洪杰
全柯丞
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

本发明涉及一种石墨烯基膜的制备方法及其在油水分离中的应用，其由氧化石墨烯与交联剂形成凝胶，干燥，在10~200千帕压强下压实后还原得到。该石墨烯基油水分离膜的制备方法简单、易行、成本低廉、可大批量工业化生产，且该膜质轻稳定，可高效循环使用。该石墨烯基油水分离膜材料可以在多种环境下高效、低能耗、超高速地分离油水混合物得到其中的油分，含水量低于200ppm，最低水含量为10ppm，根据不同油相略有差异。The invention relates to a preparation method of a graphene-based membrane and its application in oil-water separation, which is obtained by forming a gel from graphene oxide and a cross-linking agent, drying, compacting at a pressure of 10 to 200 kilopascals, and then reducing. The preparation method of the graphene-based oil-water separation membrane is simple, easy to implement, low in cost, and can be industrially produced in large quantities, and the membrane is light and stable, and can be efficiently recycled. The graphene-based oil-water separation membrane material can efficiently, low-energy, and ultra-high-speed separate the oil-water mixture to obtain the oil in various environments. The water content is less than 200ppm, and the minimum water content is 10ppm, which varies slightly according to different oil phases.

Description

A kind of preparation method of Graphene basement membrane and the application in water-oil separating thereof
Technical field
The present invention relates to a kind of preparation method of Graphene basement membrane and the application in water-oil separating thereof, belong to functional material technology, membrane separation technique and environmental protection technical field.
Background technology
Oil extraction, offshore oil leaks, and industry, life oil-polluted water etc. bring great harm to environment and the ecological balance, make oily water separation technique enjoy people to pay close attention to.At present, membrane separation technique is the effective ways to oily waste water treatment, based on organic microfiltration membranes and organic milipore filter.But because its chemical stability, heat endurance are poor, even there will be phenomenon that is swelling, that dissolve, so the use of this kind of film is very restricted.
Application number is the preparation method that application discloses a kind of graphene-based oil suction foamed composite of magnetic of 201310407309, and the method is peeled off graphite with the Hummers method improved and obtained graphite oxide; Obtain graphene oxide water solution by after graphite oxide ultrasonic disperse, in this solution, add CNT, and through suction filtration film forming; Graphene-based foamed material is obtained by hydrothermal reduction method; With graphene-based foam for carrier, prepare magnetic graphite thiazolinyl foamed composite by chemical method at its area load iron oxide.The magnetic graphite thiazolinyl foamed composite adopting the method for the invention to obtain has good absorption property to oils and organic solvent, Stability Analysis of Structures also can adopt magnetism separate method to realize reusing material, for the application of graphene-based foamed material in water-oil separating field is laid a good foundation simultaneously.
Application number be 201110066634 patent application relate to a kind of fast preparation method of graphene oxide film, take crystalline graphite powder as raw material, take flat glass as film-forming carrier, with sulfuric acid, sodium nitrate, potassium permanganate, hydrogen peroxide is preparation process material, deionized water is for preparing solvent, take nitrogen as protective gas, first in four-hole boiling flask, prepare graphene oxide solution, with salpeter solution, graphene oxide is flocculated, then film forming on flat glass, graphene oxide film is obtained through vacuum drying, film thickness is 1-2 μm, intensity is good, toughness is large, Resisting fractre intensity is good, the method technological process is short, speed is fast, processing ease, can accomplish scale production.
The technological process of the preparation method of above-mentioned prior art is all comparatively complicated, and cost is high, and the auxiliary agent added is many, and above-mentioned preparation method can not carry out continuous print water-oil separating operation, and its water-oil separating performance is not comprehensively investigated.
Summary of the invention
The object of the invention is to solve the problems of the prior art, prepare a kind of graphene-based water-oil separating film with economic, simple method, it forms gel by graphene oxide and crosslinking agent, dry, and under 10 ~ 200 kPas of pressure, after compacting, reduction obtains.
In a preferred embodiment of the invention, the preparation method of described graphene-based water-oil separating film comprises the steps:
(1) preparation of graphene oxide hydrogel: get the graphene oxide solution that 10mL concentration is 1 ~ 100mg/mL, the crosslinking agent adding 0.5mmol ~ 0.1mol, at 60 ~ 150 DEG C of reaction 4 ~ 8h, obtains graphene oxide hydrogel;
(2) preparation of graphene oxide xerogel: graphene oxide hydrogel drying process step (1) obtained, obtains graphene oxide xerogel;
(3) press mold: by graphene oxide xerogel compacting under 10 ~ 200 kPas of pressure of step (2) gained, maintains 5 ~ 50min;
(4) graphene film preparation: by the graphene oxide membrane reduction after the compacting of step (3) gained, obtain graphene film.
In a preferred embodiment of the invention, described crosslinking agent is ethylenediamine, diethylenetriamine, triethylene tetramine, N-hydroxyethyl-ethylenediamine, polymine, dithioglycol, dimercaptopropane, 1,6-ethanthiol or 2,3-diaminopropionic acid.
In a preferred embodiment of the invention, described method of reducing is any one in following two kinds:
(1), under one or more reducing agent effects in hydrazine hydrate or hydroiodic acid, vitamin C, sodium borohydride, iron chloride of the xerogel after compacting, at 0 ~ 100 DEG C, 1 ~ 120min is reduced; Or,
(2) xerogel after compacting, under inert gas shielding effect, 100 ~ 800w microwave reduction, 5 ~ 300s.
The present invention also protects this application of Graphene basement membrane in water-oil separating.Wherein, profit comprises oil phase and aqueous phase.
In a preferred embodiment of the invention, oil phase is the mixing of one or more components in oil, rape oil, gasoline, diesel oil, benzinum, cyclohexane, normal heptane, normal octane, ethyl acetate, benzene,toluene,xylene, carrene, chloroform; Wherein, oil phase accounts for 10 ~ 99.9% of oil phase and aqueous phase mixed volume.
In a preferred embodiment of the invention, aqueous phase is water, or hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, NaOH, potassium hydroxide, sodium chloride, potassium chloride, copper chloride, iron chloride, one or more solutes in copper sulphate the aqueous solution, wherein in the aqueous solution, the mass fraction of total soluble matters is 0.1 ~ 90%.
In a preferred embodiment of the invention, one or more surfactants in span 80, this dish 60, this dish 20, Tween 80, polysorbate60, polysorbas20, neopelex, S-170 are contained in oil water mixture.
The preparation method of this graphene-based water-oil separating film is simple, easy, with low cost, can mass industrialized production, and this film quality is gently stablized, and can efficient circulation use.This graphene-based water-oil separating membrane material efficient, low energy consumption in a variety of contexts, ultrahigh speed ground oil-water separation mixture can obtain wherein oil content, and water content is lower than 200ppm, and minimum water content is 10ppm, according to different oil phase slightly difference.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described
Fig. 1: the graphene-based water-oil separating film prepared in the embodiment of the present invention 2;
Fig. 2: the stereoscan photograph on the graphene-based water-oil separating film surface prepared in the embodiment of the present invention 2, clearly can see this film surface very polishing;
Fig. 3 (a): the graphene-based water-oil separating film obtained in the embodiment of the present invention 2 is in atmosphere to the contact angle photo of oil droplet, and contact angle is close to 0 o, confirm it and there is super-oleophilic matter in atmosphere;
Fig. 3 (b): the graphene-based water-oil separating film obtained in the embodiment of the present invention 2 in atmosphere to the contact angle photo of water droplet, contact angle about 95 o, confirm it and have hydrophobic property in atmosphere.
Detailed description of the invention
Below by embodiment, the present invention will be further described:
Embodiment 1
100 microlitre dithioglycols are joined in 10mL graphene oxide water solution (80mg/mL), stirs rear 70 DEG C of reaction 4h and obtain graphene oxide hydrogel, after hydrogel drying, obtain graphene oxide xerogel; Under 50 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 5min, immersed by xerogel subsequently in 85% hydrazine hydrate, 100 DEG C of reaction 30min, obtain Graphene basement membrane material; Finally, by the graphene film material surname extraction 5h in aqueous obtained, 60 DEG C of oven dry can be directly used in water-oil separating.
Embodiment 2
100 microlitre ethylenediamines are joined in 10mL graphene oxide water solution (50mg/mL), stirs rear 100 DEG C of reaction 4h and obtain graphene oxide hydrogel, after hydrogel drying, obtain graphene oxide xerogel; Under 80 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 10min, immersed by xerogel subsequently in 55% hydroiodic acid, 90 DEG C of reaction 30min, obtain Graphene basement membrane material; Finally, by the graphene film material surname extraction 5h in aqueous obtained, 60 DEG C of oven dry can be directly used in water-oil separating.
Embodiment 3
200 microlitre diethylenetriamines are joined in 10mL graphene oxide water solution (20mg/mL), stirs rear 120 DEG C of reaction 6h and obtain graphene oxide hydrogel, after hydrogel drying, obtain graphene oxide xerogel; Under 80 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 5min, immersed by xerogel subsequently in 85% hydrazine hydrate solution, 90 DEG C of reaction 10min, obtain Graphene basement membrane material; Finally, by the graphene film material surname extraction 5h in aqueous obtained, 60 DEG C of oven dry can be directly used in water-oil separating.
Embodiment 4
50 microlitre polymines are joined in 10mL graphene oxide water solution (5mg/mL), stirs rear 70 DEG C of reaction 4h and obtain graphene oxide hydrogel, after hydrogel drying, obtain graphene oxide xerogel; Under 50 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 5min, xerogel 800w microwave 60 seconds under nitrogen protection, obtains Graphene basement membrane material and can be directly used in water-oil separating subsequently.
Embodiment 5
100 microlitre dimercaptopropanes are joined in 10mL graphene oxide water solution (6mg/mL), stirs rear 95 DEG C of reaction 4h and obtain graphene oxide hydrogel, after hydrogel drying, obtain graphene oxide xerogel; Under 80 kPas of pressure, by the compacting of graphene oxide xerogel, maintain 10min, immersed by xerogel subsequently in 50mM sodium borohydride aqueous solution, 90 DEG C of reaction 30min, obtain Graphene basement membrane material; Finally, by the graphene film material surname extraction 5h in aqueous obtained, 60 DEG C of oven dry can be directly used in water-oil separating.
Embodiment 6
The graphene-based water-oil separating film that Example 2 prepares is fixed in filter; 90mL isooctane and 10mL water are mixed to form suspension, and pour on the separator put up, by diffusion barrier, water is trapped isooctane.Finally measuring water content in the isooctane obtained is 10ppm.
Embodiment 7
The graphene-based water-oil separating film that Example 2 prepares is fixed in filter; 50mL diesel oil and 50mL water are mixed to form suspension, and pour on the separator put up, by diffusion barrier, water is trapped diesel oil.Finally measuring water content in the diesel oil obtained is 15ppm.
Embodiment 8
The graphene-based water-oil separating film that Example 3 prepares is fixed in filter; 90mL toluene and 10mL8M sodium hydrate aqueous solution are mixed to form suspension, and pour on the separator put up, by diffusion barrier, sodium hydrate aqueous solution is trapped toluene.Finally measuring water content in the toluene obtained is 80ppm.
Embodiment 9
The graphene-based water-oil separating film that Example 5 prepares is fixed in filter; 40mL toluene, 40mL benzinum and 20mL water are mixed to form suspension, and pour on the separator put up, the aqueous solution is trapped by diffusion barrier for toluene and benzinum mixed solution.Finally measuring water content in the toluene and benzinum mixed solution obtained is 85ppm.
Embodiment 10
The graphene-based water-oil separating film that Example 4 prepares is fixed in filter; 40mL toluene, 10mgS-170 and 60mL water are mixed to form suspension, and pour on the separator put up, by diffusion barrier, the aqueous solution is trapped toluene.Finally measuring water content in the toluene solution obtained is 100ppm.
Embodiment 11
The graphene-based water-oil separating film that Example 2 prepares is fixed in filter; 80mL ethyl acetate, 10mg neopelex and 20mL water are mixed to form suspension, and pour on the separator put up, by diffusion barrier, the aqueous solution is trapped ethyl acetate.Finally measuring water content in the ethyl acetate solution obtained is 50ppm.
Embodiment 12
The graphene-based water-oil separating film that Example 2 prepares is fixed in filter; 30mL ethyl acetate, 30mL normal octane, 10mg neopelex, 10mgSpan80 and 40mL water are mixed to form suspension, pour on the separator put up, the aqueous solution is trapped by diffusion barrier for ethyl acetate and normal octane mixed solution.Finally measuring water content in the ethyl acetate and normal octane mixed solution obtained is 90ppm.
Above embodiment display and describe general principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; instead of limit the scope of the invention by any way; without departing from the scope of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.

Claims (8)

1.一种石墨烯基膜的制备方法，其特征在于，具体包括如下步骤： 1. a preparation method of graphene-based film, is characterized in that, specifically comprises the steps: （1）氧化石墨烯水凝胶的制备：取10mL浓度为1~100mg/mL的氧化石墨烯溶液，加入0.5mmol~0.1mol的交联剂在60~150℃反应4~8h，得到氧化石墨烯水凝胶； (1) Preparation of graphene oxide hydrogel: Take 10 mL of graphene oxide solution with a concentration of 1-100 mg/mL, add 0.5 mmol-0.1 mol of cross-linking agent and react at 60-150 °C for 4-8 hours to obtain graphite oxide Alkene hydrogel; （2）氧化石墨烯干凝胶的制备：将步骤（1）得到的氧化石墨烯水凝胶干燥处理，得到氧化石墨烯干凝胶； (2) Preparation of graphene oxide xerogel: drying the graphene oxide hydrogel obtained in step (1) to obtain graphene oxide xerogel; （3）压膜：将步骤（2）所得的氧化石墨烯干凝胶在10~200千帕压强下压实，维持5~50min； (3) Film pressing: compact the graphene oxide xerogel obtained in step (2) under a pressure of 10-200 kPa for 5-50 minutes; （4）石墨烯膜制备：将步骤（3）所得的压实后的氧化石墨烯膜还原，得到石墨烯基膜。 (4) Preparation of graphene film: reducing the compacted graphene oxide film obtained in step (3) to obtain a graphene-based film. 2.根据权利要求1所述的制备方法，其特征在于，所述交联剂为乙二胺、二乙烯三胺、三乙烯四胺、N-羟乙基乙二胺、聚乙烯亚胺、乙二硫醇、丙二硫醇、1,6-己二硫醇或2,3-二氨基丙酸。 2. preparation method according to claim 1, is characterized in that, described linking agent is ethylenediamine, diethylenetriamine, triethylenetetramine, N-hydroxyethylethylenediamine, polyethyleneimine, Ethanedithiol, propanedithiol, 1,6-hexanedithiol, or 2,3-diaminopropionic acid. 3.根据权利要求1所述的制备方法，其特征在于，所述的还原方法为以下两种中的任意一种： 3. preparation method according to claim 1, is characterized in that, described reduction method is any one in following two kinds: （1）压实后的干凝胶在水合肼或氢碘酸、维生素C、硼氢化钠、氯化铁中的一种或多种还原剂作用下，在0~100℃下还原1~120min；或， (1) The compacted xerogel is reduced at 0-100°C for 1-120 min under the action of one or more reducing agents in hydrazine hydrate or hydroiodic acid, vitamin C, sodium borohydride, and ferric chloride ;or, （2）压实后的干凝胶，在惰性气体保护作用下，100~800W微波还原5~300s。 (2) The compacted dry gel is reduced by 100~800W microwave for 5~300s under the protection of inert gas. 4.根据权利要求1-3之一所述的制备方法制备得到的石墨烯基膜。 4. The graphene-based film prepared according to the preparation method described in one of claims 1-3. 5.根据权利要求4所述的石墨烯基膜在油水分离中的应用。 5. the application of graphene-based membrane according to claim 4 in oil-water separation. 6.根据权利要求5所述的应用，其特征在于，油水包括油相和水相，其中油相为石油、菜油、汽油、柴油、石油醚、环己烷、正庚烷、正辛烷、乙酸乙酯、苯、甲苯、二甲苯、二氯甲烷、氯仿中的一种或多种组分的混合；油相占油相和水相混合体积的10~99.99%。 6. application according to claim 5, is characterized in that, oil-water comprises oil phase and water phase, and wherein oil phase is petroleum, rapeseed oil, gasoline, diesel oil, sherwood oil, hexanaphthene, n-heptane, n-octane, A mixture of one or more components of ethyl acetate, benzene, toluene, xylene, methylene chloride, and chloroform; the oil phase accounts for 10~99.99% of the volume of the mixture of the oil phase and the water phase. 7.根据权利要求6所述的应用，其特征在于，水相为水，或盐酸、硫酸、硝酸、磷酸、氢氧化钠、氢氧化钾、氯化钠、氯化钾、氯化铜、氯化铁、硫酸铜中的一种或多种溶质的水溶液，其中水溶液中总溶质的质量分数为0.1~90%。 7. application according to claim 6, is characterized in that, water phase is water, or hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, sodium hydroxide, potassium hydroxide, sodium chloride, potassium chloride, cupric chloride, chlorine An aqueous solution of one or more solutes in iron oxide and copper sulfate, wherein the mass fraction of the total solutes in the aqueous solution is 0.1-90%. 8.根据权利要求5-7之一所述的应用，其特征在于，油水混合物中含有斯盘80、斯盘60、斯盘20、吐温80、吐温60、吐温20、十二烷基苯磺酸钠、S-170中的一种或多种表面活性剂。 8. The application according to any one of claims 5-7, characterized in that the oil-water mixture contains Span 80, Span 60, Span 20, Tween 80, Tween 60, Tween 20, dodecane Sodium benzene sulfonate, one or more surfactants in S-170.
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