CN101073773A

CN101073773A - Ferro-carbon composite nano-catalyst for microwave water treatment and its production

Info

Publication number: CN101073773A
Application number: CN 200710052555
Authority: CN
Inventors: 肖咪; 王毓楠
Original assignee: Central China Normal University
Current assignee: Central China Normal University
Priority date: 2007-06-26
Filing date: 2007-06-26
Publication date: 2007-11-21
Anticipated expiration: 2027-06-26
Also published as: CN100522353C

Abstract

The invention relates to an iron-carbon composite nano catalyst for microwave water treatment and a preparation method thereof, belonging to the technical field of preparation of microwave water treatment catalysts. The main composition of the catalyst is iron source and carbon source, and the mass ratio of iron source and carbon source is 10-1:1. Wherein said iron source is nanometer zero valent iron or nanometer ferric oxide; said carbon source is carbon nanotube or carbon nanofiber material. The preparation method is: use carbon source, iron source and polytetrafluoroethylene emulsion as raw materials, mix them evenly according to the composition ratio, and dry them at room temperature under the protection of nitrogen after molding to obtain iron-carbon composite nano-catalysis materials that can be used for microwave water treatment. . The iron-carbon composite nano catalytic material synthesized by the method of the invention has high catalytic efficiency, simple synthesis route, easy control of the whole process, and is carried out at normal temperature and pressure, which meets the needs of actual microwave water treatment technology.

Description

Be used for ferro-carbon composite nano-catalyst of microwave water treatment and preparation method thereof

Technical field

The present invention relates to a kind of preparation method of ferro-carbon composite nano-catalyst, belong to microwave water treatment catalyst preparation technical field.

Background technology

Along with China's rapid economy development, a series of association problems such as resource and energy shortage, environmental pollution, disease propagation become increasingly conspicuous.How to eliminate and avoid polluting, the effective way of seeking out purification of water quality becomes the focus of the current concern of people.In recent years, the microwave water technology is one of trend of present water treatment development both domestic and external, and its feature is an efficient energy-saving, non-secondary pollution, and capital expenditure is economized, operating cost is low, and it is good to handle back water quality.Wherein, select for use the catalyst of which kind of microwave water treatment most important for the efficient of microwave water treatment, in water technology,, thereby be used for treatment of Organic Wastewater and even contaminated soil reparation because Zero-valent Iron has reduction to various chlorinatedorganics, nitro compound and heavy metal etc. in the water; And because carbon class material such as active carbon particle, activated carbon fibers etc. have bigger specific area, and organic pollution in the water or heavy metal ion are had stronger suction-operated, thereby particularly use in the advanced treating technology in water treatment.

Have not yet to see patent report about the preparation of preparation iron carbon composite microwave water treatment nano-catalyst material, domestic patent about the microwave inducing catalyst material only limits to prepare modified aluminas or is compounded with barium ferrite and the foam-like material of RESEARCH OF PYROCARBON, rather than iron carbon nano-composite material, as prepare the modified alumina catalyst (CN1559670A) that can be used for microwave-induced oxidation process after adopting commercial alumina activation drying and roasting, adopt soluble barium salt and molysite, compound with gelatin polymer part with network structure, pyrolysis, calcining, obtain being compounded with the foam-like material of barium ferrite and RESEARCH OF PYROCARBON, be used for microwave degradation water organic pollution (CN1765494A).The preparation technology who adopts in these patents is complicated, and energy consumption and cost are higher.

The present invention utilizes nanometer iron, nano-sized carbon and high molecule emulsion polymerization prepared in reaction to be used for the ferro-carbon composite nano-catalyst material of microwave water treatment, and technology is simple, and cost is low, is convenient to further extension and produces, and has broad application prospects in water treatment field.

Summary of the invention

The object of the present invention is to provide a kind of ferro-carbon composite nano-catalyst and preparation method of microwave water treatment.Be base stock directly, add the high molecular polymer polymerisation, prepare the nano composite material of microwave absorbing property and catalytic performance preferably with nano zero valence iron or nanometer di-iron trioxide and carbon nanomaterial.

A kind of ferro-carbon composite nano-catalyst that is used for the microwave water treatment of the present invention, this catalyst mainly consist of source of iron and carbon source, source of iron and carbon source mass ratio are 10～1: 1, wherein said source of iron is nano zero valence iron or nanometer di-iron trioxide; Described carbon source is CNT or carbon nano-fiber material.

The preparation method's step that is used for the ferro-carbon composite nano-catalyst of microwave water treatment of the present invention is:

Step 1, take by weighing source of iron and carbon source joins in the container, the mass ratio of source of iron and carbon source is 10～1: 1, mixes, and described source of iron is nano zero valence iron or nanometer di-iron trioxide, and described carbon source is CNT or carbon nano-fiber material;

Step 2, in the mixture of step 1 gained, add macromolecular compound emulsion and surfactant, wherein the quality of macromolecular compound emulsion accounts for 5～10% of source of iron and carbon source gross mass, the quality of surfactant accounts for 2～10% of source of iron and carbon source gross mass, stirs;

Step 3, with the mixture of step 2 gained air drying 1～2 hour under nitrogen protection, obtain the sticking shape material of black;

Step 4, the sticking shape material of step 3 gained is done slabbing or graininess, 60～80 degrees centigrade of control temperature dry 3～10 hours down promptly obtain ferro-carbon composite nano-catalyst.

Source of iron described in the step 1 is nano zero valence iron or nanometer di-iron trioxide; Described carbon source is CNT or carbon nano-fiber material.

Surfactant described in the step 2 is polyethylene glycol, soluble starch, polystyrene, dodecyl sodium sulfate, Cetrimide, tween, sulfamic acid sodium, sulfamic acid potassium, asccharin or 1,4 butynediols; Described macromolecular compound emulsion is polyvinyl alcohol emulsion, polyvinyl acetate emulsion, ptfe emulsion, polyacrylic acid emulsion, polyaminoester emulsion or epoxy resin.

Advantage of the present invention:

1, synthetic route is simple, and whole technical process is controlled easily, and carries out at normal temperatures and pressures, the needs of realistic production;

2, source of iron and carbon source are uniformly dispersed in the He Cheng nano-composite catalyst material;

3, He Cheng nano-composite catalyst material has microwave absorbing property preferably, has broad application prospects in water treatment field.

Description of drawings

Fig. 1 (a) is the scanning electron microscope diagram of 5,000 times of amplifications of the ferro-carbon composite nano material for preparing of the present invention;

Fig. 1 (b) is the scanning electron microscope diagram of 10,000 5 thousand times of amplifications of the ferro-carbon composite nano material for preparing of the present invention;

Fig. 2 is the ferro-carbon composite nano material transmission electron microscope figure that the present invention prepares;

Fig. 3 is the powder crystal X-ray diffractogram of the ferro-carbon composite nano material for preparing of the present invention

Fig. 4 is the ferro-carbon composite nano material energy dispersive x ray analysis figure that the present invention prepares;

Fig. 5 is that the ferro-carbon composite nano material for preparing of the present invention is at microwave system catalytic degradation waste water from dyestuff figure.

The specific embodiment

Embodiment 1

Preparation is used for the ferro-carbon composite nano material catalyst of microwave water treatment, and preparation process is:

Step 1, take by weighing nano zero valence iron 50g and 5g CNT in container, mix;

Step 2, in the mixture of step 1 gained, add 5.5g ptfe emulsion and 5g dodecyl sodium sulfate, stir;

Step 3, at the mixture of step 2 gained air drying 2 hours under nitrogen protection, obtain the sticking shape material of black.

Step 4, do slabbing or graininess at the sticking shape material of step 3 gained, 70 degrees centigrade of control temperature dry 8 hours down can obtain the nano combined nano-catalyst material of iron carbon.

Embodiment 2

Step 1, take by weighing nano zero valence iron 50g and 50g carbon nano-fiber in container, mix;

Step 2, in the mixture of step 1 gained, add 10g ptfe emulsion and 10g polyethylene glycol, stir;

Step 4, do slabbing or graininess at the sticking shape material of step 3 gained, 80 degrees centigrade of control temperature dry 10 hours down can obtain the nano combined nano-catalyst material of iron carbon.

Embodiment 3

Step 1, take by weighing nano zero valence iron 40g and 10g CNT in container, mix;

Step 2, in the mixture of step 1 gained, add 10g ptfe emulsion and 5g polyethylene glycol, stir;

Step 4, do slabbing or graininess at the sticking shape material of step 3 gained, 70 degrees centigrade of control temperature dry 10 hours down can obtain the nano combined nano-catalyst material of iron carbon.

Embodiment 4

Step 1, take by weighing nanometer di-iron trioxide 50g and 30g carbon nano-fiber in container, mix;

Step 2, in the mixture of step 1 gained, add 25g ptfe emulsion and 4g polyethylene glycol, stir;

Step 4, do slabbing or graininess at the sticking shape material of step 3 gained, 60 degrees centigrade of control temperature dry 10 hours down can obtain the nano combined nano-catalyst material of iron carbon.

Embodiment 5

Step 1, take by weighing nanometer di-iron trioxide 50g and 10g CNT in container, mix;

Step 2, in the mixture of step 1 gained, add 6g polyvinyl alcohol emulsion and 2g tween, stir;

Step 4, do slabbing or graininess at the sticking shape material of step 3 gained, 60 degrees centigrade of control temperature dry 10 hours down can obtain the nano combined nano-catalyst material of iron carbon of black.

Embodiment 6

Step 2, in the mixture of step 1 gained, add 7g polyaminoester emulsion and 3g Cetrimide, stir;

Gained sample (catalyst of forming with nano zero valence iron and CNT is an example) is observed through the scanning electron microscope diagram (JSM-5600) of 5,000 times of amplifications and (is seen Fig. 1 a), the composite nano-catalyst material surface has loose structure, and the scanning electron microscope diagram of 10,000 5 thousand times of amplifications (JSM-5600) observed result (seeing Fig. 1 b) and transmission electron microscope figure (Fig. 2) illustrate that nano zero valence iron and even carbon nanotube are scattered in the sample.The gained sample is tested through XRD, the characteristic peak of (see figure 3) is identical with the peak value of iron (JCPDS3-1050), polytetrafluoroethylene (PTFE) (JCPDS 47-2217), CNT (JCPDS 74-444) respectively in the diffracting spectrum, illustrative material has iron, carbon and polytetrafluoroethylene (PTFE) to constitute, and this energy dispersive x ray analysis collection of illustrative plates (see figure 4) with sample is consistent.The gained sample under microwave to waste water from dyestuff in rhodamine B good catalytic degradation effect (see figure 5) is arranged.

Claims

1. An iron-carbon composite nano-catalyst for microwave water treatment, characterized in that: the components of the catalyst include an iron source and a carbon source, and the mass ratio of the iron source and the carbon source is 10-1:1.

2. The iron-carbon composite nano-catalyst for microwave water treatment according to claim 1, characterized in that: said iron source is nano-zero valent iron or nano-ferric oxide.

3. The iron-carbon composite nanocatalyst for microwave water treatment according to claim 1, characterized in that: the carbon source is carbon nanotube or carbon nanofiber material.

4. The preparation method of the iron-carbon composite nano-catalyst for microwave water treatment according to claim 1, characterized in that the preparation steps are:

Step 1. Weigh the iron source and the carbon source and add them to the container, the mass ratio of the iron source and the carbon source is 10-1:1, and mix evenly;

Step 2, add polymer compound emulsion and surfactant in the mixture of step 1 gained, wherein the quality of polymer compound emulsion accounts for 10～50% of the total mass of iron source and carbon source, the quality of surfactant accounts for iron source and carbon source 2-10% of the total mass of carbon source, stir evenly;

Step 3, drying the mixture obtained in step 2 at room temperature under the protection of nitrogen for 1 to 2 hours to obtain a black sticky material;

Step 4, making the viscous material obtained in step 3 into flakes or granules, and drying at a controlled temperature of 60-80 degrees Celsius for 3-10 hours to obtain an iron-carbon composite nano-catalyst.

5. The method for preparing an iron-carbon composite nanocatalyst for microwave water treatment as claimed in claim 4, wherein said surfactant is polyethylene glycol, soluble starch, polystyrene, dodecane Sodium sulfamate, bromide, Tween, sodium sulfamate, potassium sulfamate, saccharin or 1,4 butynediol.

6. The preparation method of iron-carbon composite nano-catalyst for microwave water treatment as claimed in claim 4, characterized in that: the polymer compound emulsion is polyvinyl alcohol emulsion, polyvinyl acetate emulsion, polytetrafluoroethylene Emulsion, Polyacrylic Emulsion, Polyurethane Emulsion or Epoxy.