CN102908908A - Method for modifying modified ceramic microfiltration membrane by adopting graphite oxide - Google Patents
Method for modifying modified ceramic microfiltration membrane by adopting graphite oxide Download PDFInfo
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Abstract
The invention discloses a method for modifying a modified ceramic microfiltration membrane by adopting graphite oxide, comprising the steps of preparing a modified solution, namely a graphite oxide dispersed water solution, immersing and coating a ceramic microfiltration membrane in vacuum and carrying out drying treatment to prepare the graphite oxide modified ceramic microfiltration membrane. According to the method, the separation efficiency of the ceramic microfiltration membrane is obviously improved and the acid and alkali resisting performance is effectively improved, so that good separation effect is obtained, and the service life of the ceramic microfiltration membrane is prolonged. Furthermore, the method has the advantages of simple process, low cost, green environmental friendliness and easily-controlled operation condition, and is good for being further popularized and applied.
Description
Technical field
The present invention relates to the ceramic material technical field, relate in particular to the method for ceramic micro filter film being carried out modification.
Background technology
Compare with other separating technology, it is a kind of relatively simple, low separating technology of power consumption that film separates.Film separates by membrane module to be realized, its core is filter membrane.Compare with organic film, the advantages such as ceramic filter membrane has heat endurance and chemical stability is good, mechanical strength is high, easy regeneration, easily cleaning, easy-regulating, have a wide range of applications in fields such as food, beverage (membrane filtration), medical and health (film degerming), petrochemical industry (hydrogenation, dehydrogenation), biotechnology (high temperature degerming), environmental project (such as the purification of vehicle exhaust) and novel energies (separation hydrogen), especially in the environment that relates to HTHP and corrosion, has the unrivaled advantage of other membrane material.
Yet, continuous expansion along with the ceramic filter membrane application, its applied environment is day by day complicated and changeable, need ceramic filter membrane to satisfy higher requirement, also so that ceramic filter membrane research and application process convexity show low such as separative efficiency, in key issue such as use operating process performance unstable (resistance to acids and bases was poor when especially film separated acidity or alkaline solution) etc., cause its serviceability and separating effect to be difficult to practical requirement, service life is shorter, thereby has affected further promotion and application.
At present, for improving the performance of ceramic filter membrane, prior art realizes by ceramic filter membrane is carried out modification mostly.Modification to ceramic filter membrane can be divided into membrane surface modification and fenestra modifying inner surface, mainly concentrate at present the latter, to be deposited on as the second component of modification the hole inwall of original membrane by homogeneous precipitation method, complexing and alkoxide hydrolysis, original position method of formation, or with the hydroxyl generation chemical reaction of second component and original membrane material grain surface and be bonded in the hole inwall, thereby make ceramic filter membrane after the modification have less aperture and separative efficiency or catalytic performance are higher.Yet along with the fast development that ceramic filter membrane is used, present existing modification technology still can not solve existing problem well, and not only serviceability and separative efficiency are difficult to reach requirement, and complex process, manufacturing cost are high.For this reason, how ceramic filter membrane is carried out effective modification with practical requirement, become the current pressing problem of needing solution badly.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method that adopts graphene oxide modification ceramic micro filter film is provided, by improving the hydrophilic or hydrophobicity performance of ceramic micro filter film, to significantly improve the ceramic micro filter membrane separation efficiency, and Effective Raise acid-proof alkaline, thereby obtain good separating effect, and greatly prolong the service life of ceramic micro filter film.
Purpose of the present invention is achieved by the following technical programs:
A kind of method that adopts graphene oxide modification ceramic micro filter film provided by the invention may further comprise the steps:
(1) preparation of modified solution: take graphite such as crystalline flake graphite, expansible graphite, micro crystal graphite etc. as raw material, adopt the standby graphene oxide aqueous dispersion of wet-chemical oxidizing process such as Staudenmaier method, Brodie method or Hummers legal system, the solid content of described graphene oxide aqueous dispersion is 0.01～0.1wt%, is advisable with 0.02～0.05wt%;
(2) modification is processed: ceramic micro filter film is placed reactor and immerses described graphene oxide aqueous dispersion fully, and the mode that adopts vacuum impregnation to apply is carried out the graphene oxide modification to ceramic micro filter film;
(3) heat treatment of modified ceramic microfiltration membranes: the ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, is cooled to room temperature after the oven dry, namely obtains graphene oxide modification ceramic micro filter film.
Further, the particle diameter of graphene oxide is 50～100nm in the step of the present invention (1).In the described step (2) vacuum be-0.6～-1.0bar, the processing time is 1～2h.The temperature of drying and processing is 90～105 ℃ in the described step (3), and drying time is 8～12h.
In the such scheme, ceramic micro filter film of the present invention is aluminium oxide, titanium oxide, zirconia, quartz, mullite, cordierite, clayey ceramic micro filter film.
The present invention has following beneficial effect:
The present invention is take graphene oxide as modified material, by carrying out surface modified to ceramic micro filter film, improved the hydrophilic or hydrophobicity performance of ceramic micro filter film, significantly improved the ceramic micro filter membrane separation efficiency, simultaneously Effective Raise acid-proof alkaline, thereby obtain good separating effect, and help to improve the service life of ceramic micro filter film.In addition, the present invention has the advantages such as technique is simple, with low cost, environmental protection, the easy control of operating condition, is conducive to further promotion and application.
Description of drawings
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing:
Fig. 1 is the process flow diagram of the embodiment of the invention.
The specific embodiment
Embodiment one:
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present embodiment, as shown in Figure 1, its step is as follows:
(1) preparation of modified solution
Take crystalline flake graphite as raw material, adopt the synthetic preparation of Staudenmaier method graphene oxide aqueous dispersion; By clean to separate, the ultrasonic wave pulverization process, the graphene oxide aqueous dispersion that obtains the graphene oxide particle diameter and be 60nm, solution solid content and be 0.05wt% and be uniformly dispersed stable;
(2) modification is processed
The aluminum oxide ceramic micro filter film is placed reactor and immerses the graphene oxide aqueous dispersion fully, the mode that adopts vacuum impregnation to apply, namely vacuumize after the sealing, reach-keep 1h after the vacuum of 0.8bar, ceramic micro filter film is carried out the graphene oxide modification;
(3) heat treatment of modified ceramic microfiltration membranes
Ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, dries 8h under 105 ℃ of temperature, is cooled to room temperature, namely obtains graphene oxide modification aluminum oxide ceramic micro filter film.
Embodiment two:
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present embodiment, as shown in Figure 1, its step is as follows:
(1) preparation of modified solution
Take expansible graphite as raw material, adopt the synthetic preparation of Brodie method graphene oxide aqueous dispersion; By clean to separate, the ultrasonic wave pulverization process, the graphene oxide aqueous dispersion that obtains the graphene oxide particle diameter and be 80nm, solution solid content and be 0.05wt% and be uniformly dispersed stable;
(2) modification is processed
Titanium oxide matter ceramic micro filter film is placed reactor and immerses the graphene oxide aqueous dispersion fully, the mode that adopts vacuum impregnation to apply, namely vacuumize after the sealing, reach-keep 1.5h after the 0.8bar vacuum, ceramic micro filter film is carried out the graphene oxide modification;
(3) heat treatment of modified ceramic microfiltration membranes
Ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, dries 10h under 100 ℃ of temperature, is cooled to room temperature, namely obtains graphene oxide modification titanium oxide matter ceramic micro filter film.
Embodiment three:
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present embodiment, as shown in Figure 1, its step is as follows:
(1) preparation of modified solution
Take micro crystal graphite as raw material, adopt the synthetic preparation of Hummers method graphene oxide aqueous dispersion; By clean to separate, the ultrasonic wave pulverization process, the graphene oxide aqueous dispersion that obtains the graphene oxide particle diameter and be 50nm, solution solid content and be 0.02wt% and be uniformly dispersed stable;
(2) modification is processed
The zirconium oxide ceramic micro filter film is placed reactor and immerses the graphene oxide aqueous dispersion fully, the mode that adopts vacuum impregnation to apply, namely vacuumize after the sealing, reach-keep 2h after the vacuum of 0.6bar, ceramic micro filter film is carried out the graphene oxide modification;
(3) heat treatment of modified ceramic microfiltration membranes
Ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, dries 12h under 95 ℃ of temperature, is cooled to room temperature, namely obtains graphene oxide modification zirconium oxide ceramic micro filter film.
Embodiment four:
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present embodiment, as shown in Figure 1, its step is as follows:
(1) preparation of modified solution
Take crystalline flake graphite as raw material, adopt the synthetic preparation of Hummers method graphene oxide aqueous dispersion; By clean to separate, the ultrasonic wave pulverization process, the graphene oxide aqueous dispersion that obtains the graphene oxide particle diameter and be 70nm, solution solid content and be 0.05wt% and be uniformly dispersed stable;
(2) modification is processed
The quartziferous ceramic micro filter film is placed reactor and immerses the graphene oxide aqueous dispersion fully, the mode that adopts vacuum impregnation to apply, namely vacuumize after the sealing, reach-keep 1.5h after the vacuum of 0.8bar, ceramic micro filter film is carried out the graphene oxide modification;
(3) heat treatment of modified ceramic microfiltration membranes
Ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, dries 10h under 100 ℃ of temperature, is cooled to room temperature, namely obtains graphene oxide modification quartziferous ceramic micro filter film.
Embodiment five:
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present embodiment, as shown in Figure 1, its step is as follows:
(1) preparation of modified solution
Take expansible graphite as raw material, adopt the synthetic preparation of Hummers method graphene oxide aqueous dispersion; By clean to separate, the ultrasonic wave pulverization process, the graphene oxide aqueous dispersion that obtains the graphene oxide particle diameter and be 100nm, solution solid content and be 0.05wt% and be uniformly dispersed stable;
(2) modification is processed
The mullite ceramic micro filter film is placed reactor and immerses the graphene oxide aqueous dispersion fully, the mode that adopts vacuum impregnation to apply, namely vacuumize after the sealing, reach-keep 1h after the vacuum of 1.0bar, ceramic micro filter film is carried out the graphene oxide modification;
(3) heat treatment of modified ceramic microfiltration membranes
Ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, dries 12h under 90 ℃ of temperature, is cooled to room temperature, namely obtains graphene oxide modification mullite ceramic micro filter film.
Embodiment six:
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present embodiment, as shown in Figure 1, its step is as follows:
(1) preparation of modified solution
Take micro crystal graphite as raw material, adopt the synthetic preparation of Staudenmaier method graphene oxide aqueous dispersion; By clean to separate, the ultrasonic wave pulverization process, the graphene oxide aqueous dispersion that obtains the graphene oxide particle diameter and be 50nm, solution solid content and be 0.02wt% and be uniformly dispersed stable;
(2) modification is processed
The cordierite ceramic microfiltration membranes is placed reactor and immerses the graphene oxide aqueous dispersion fully, the mode that adopts vacuum impregnation to apply, namely vacuumize after the sealing, reach-keep 1.5h after the vacuum of 0.8bar, ceramic micro filter film is carried out the graphene oxide modification;
(3) heat treatment of modified ceramic microfiltration membranes
Ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, dries 8h under 105 ℃ of temperature, is cooled to room temperature, namely obtains graphene oxide modification cordierite ceramic microfiltration membranes.
The performance indications of above-described embodiment one～six graphene oxide modification ceramic micro filter film are as shown in table 1.
The performance indications of table 1 embodiment one～six graphene oxide modification ceramic micro filter film
Remarks: * is with respect to unmodified ceramic micro filter film, the percentage that its pure water permeation flux of embodiment of the invention graphene oxide modification ceramic micro filter film improves.
The result shows, embodiment of the invention graphene oxide modification ceramic micro filter membrane separation efficiency and acid-proof alkaline have all had significant raising, thereby have good separating effect, and help to improve the service life of ceramic micro filter film.
A kind of method that adopts graphene oxide modification ceramic micro filter film of the present invention, its technological parameter is not limited to the above-mentioned embodiment that enumerates.
Claims (6)
1. method that adopts graphene oxide modification ceramic micro filter film is characterized in that may further comprise the steps:
(1) preparation of modified solution: take graphite as raw material, adopt the wet-chemical oxidizing process to prepare the graphene oxide aqueous dispersion, the solid content of described graphene oxide aqueous dispersion is 0.01～0.1wt%;
(2) modification is processed: ceramic micro filter film is placed reactor and immerses described graphene oxide aqueous dispersion fully, and the mode that adopts vacuum impregnation to apply is carried out the graphene oxide modification to ceramic micro filter film;
(3) heat treatment of modified ceramic microfiltration membranes: the ceramic micro filter film after vacuum impregnation applied takes out and places baking oven, is cooled to room temperature after the oven dry, namely obtains graphene oxide modification ceramic micro filter film.
2. the method for employing graphene oxide modification ceramic micro filter film according to claim 1 is characterized in that: the solid content of graphene oxide aqueous dispersion is 0.02～0.05wt% in the described step (1).
3. the method for employing graphene oxide modification ceramic micro filter film according to claim 1 and 2 is characterized in that: the particle diameter of graphene oxide is 50～100nm in the described step (1).
4. the method for employing graphene oxide modification ceramic micro filter film according to claim 1 is characterized in that: in the described step (2) vacuum be-0.6～-1.0bar, the processing time is 1～2h.
5. the method for employing graphene oxide modification ceramic micro filter film according to claim 1 is characterized in that: the temperature of drying and processing is 90～105 ℃ in the described step (3), and drying time is 8～12h.
6. the method for employing graphene oxide modification ceramic micro filter film according to claim 1, it is characterized in that: described ceramic micro filter film is aluminium oxide, titanium oxide, zirconia, quartz, mullite, cordierite, clayey ceramic micro filter film.
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