CN102774837A - Method for preparing activated carbon by taking ionic liquid as activator - Google Patents

Abstract

The invention discloses a method for preparing activated carbon by taking ionic liquid as an activator, which is used for preparing high-specific-surface-area activated carbon by taking ionic liquid as an activator with a wood or bamboo raw material. The iodine sorption value of the activated carbon prepared by using the method disclosed by the invention can reach 1360-1870 mg/g, and the specific surface area of the activated carbon reaches 2580-3650 m<2>/g; the activated carbon is less in activator consumption and environment-friendly, and has simple requirements on equipment; and the problem that the traditional chemical methods for preparing activated carbon is implemented by taking strong acids (H2SO4 and H3PO4) and strong alkalis (KOH and NaOH) and the like as activators, so that the pollution to the environment is heavy, and the corrosion on equipment is serious, and the like is avoided, therefore, the method disclosed by the invention has significant economic and social benefits.

Description

A kind of is that acvator prepares process of active carbon with the ionic liquid

Technical field

The invention belongs to charcoal sorbing material field, being specifically related to a kind of is that acvator prepares process of active carbon with the ionic liquid.

Background technology

Gac is a kind of particle and powder of carbonaceousmaterial, the hydrophobic adsorbent that mainly to be biological organic substance (like coal, oil, pitch, wood chip, shell etc.) obtain through charing and activation.Because gac has flourishing pore structure and huge specific surface area, it has absorption, katalysis, and material is in its hole accumulated, and keeps physics, chemical characteristics such as stability.Can use under HTHP with multiple solvent in the pH value scope widely.At present, gac has been widely used in every field such as environment protection, chemical industry, food-processing, hydrometallurgy, medicine are refining, military chemistry protection, is national economy and national defense construction and the requisite product of people's daily life.But, adopt strong acid (H when the traditional chemical legal system is equipped with gac ₂SO ₄, H ₃PO ₄), highly basic (KOH, NaOH), ZnCl ₂Deng being that acvator is big for environment pollution, serious to equipment corrosion, activator level is big, cost is high.Therefore, the technology of a kind of eco-friendly preparation gac of exploitation searching becomes the focus of present people's research.

Summary of the invention

The object of the present invention is to provide a kind of is that acvator prepares process of active carbon with the ionic liquid, adopts the activated carbon-iodine adsorptive value of this method preparation can reach 1360 ~ 1870mg/g, and specific surface area reaches 2580 ~ 3650m ²/ g; And the activated carbon activator consumption is few, environmental friendliness, simple to equipment requirements; Avoid the traditional chemical legal system to be equipped with gac and adopted strong acid (H ₂SO ₄, H ₃PO ₄), highly basic (KOH, NaOH), ZnCl ₂Deng be acvator big for environment pollution, to problem such as equipment corrosion is serious, have remarkable economical and social benefit.

For realizing above-mentioned purpose, the present invention adopts following technical scheme:

A kind of is that acvator prepares process of active carbon with the ionic liquid, and wooden or bamboo raw material is the gac that acvator prepares high-specific surface area with the ionic liquid.

Said method comprising the steps of:

(1) wooden or bamboo raw material are pulverized, screening filters out the raw material that particle size range is 0.5-2.5mm, puts into air dry oven, under 105 ℃, dries to constant weight;

(2) be 50:1 ~ 10:1 thorough mixing by mass ratio at room temperature, and flood 2 ~ 5h the raw material and the ionic liquid of step (1);

(3) will be in the raw material after step (2) is handled be packed stainless steel tubular type reactor drum into, and be installed on the tube type resistance furnace, in stainless steel tubular type reactor drum, feed nitrogen then; Speed with 10-30 ℃/min is warming up to 200-400 ℃, and insulation 0.5-3h; Then the speed with 5 ~ 20 ℃/min is warming up to 600-900 ℃, and insulation 1-3h; After reaction finished, room temperature to be naturally cooled to stopped logical nitrogen;

(4) product of step (3) is put into zero(ppm) water and soak, heated and boiled, washing, when pH=7, drying promptly obtains gac.

Described ionic liquid is to contain in the ionic liquid of hexafluoro-phosphate radical or tetrafluoroborate one or several.

Beneficial effect of the present invention: adopt the activated carbon-iodine adsorptive value of this method preparation can reach 1360 ~ 1870mg/g, specific surface area reaches 2580 ~ 3650m ²/ g; And the activated carbon activator consumption is few, environmental friendliness, simple to equipment requirements; Avoid the traditional chemical legal system to be equipped with gac and adopted strong acid (H ₂SO ₄, H ₃PO ₄), highly basic (KOH, NaOH), ZnCl ₂Deng be acvator big for environment pollution, to problem such as equipment corrosion is serious, have remarkable economical and social benefit.

Description of drawings

Fig. 1 is the adsorption isotherm line chart of gac.

Fig. 2 is that scheme respectively in the aperture of gac.

Embodiment

Embodiment 1

(1) wooden or bamboo raw material are pulverized, screening filters out the raw material that particle size range is 0.5-2.5mm, puts into air dry oven, under 105 ℃, dries to constant weight;

(2) be the 50:1 thorough mixing by mass ratio at room temperature with the raw material and the ionic liquid of step (1), and dipping 5h;

(3) will be in the raw material after step (2) is handled be packed stainless steel tubular type reactor drum into, and be installed on the tube type resistance furnace, in stainless steel tubular type reactor drum, feed nitrogen then; Speed with 10 ℃/min is warming up to 200 ℃, and insulation 1h; Then the speed with 10 ℃/min is warming up to 600 ℃, and insulation 3h; After reaction finished, room temperature to be naturally cooled to stopped logical nitrogen;

(4) product of step (3) is put into zero(ppm) water and soak, heated and boiled, washing, when pH=7, drying promptly obtains gac.

Described ionic liquid is [Bmim] BF ₄

Embodiment 2

(1) wooden or bamboo raw material are pulverized, screening filters out the raw material that particle size range is 0.5-2.5mm, puts into air dry oven, under 105 ℃, dries to constant weight;

(2) be the 20:1 thorough mixing by mass ratio at room temperature, and flood 2 ~ 5h the raw material and the ionic liquid of step (1);

(3) will be in the raw material after step (2) is handled be packed stainless steel tubular type reactor drum into, and be installed on the tube type resistance furnace, in stainless steel tubular type reactor drum, feed nitrogen then; Speed with 20 ℃/min is warming up to 350 ℃, and insulation 2h; Then the speed with 1 ℃/min is warming up to 700 ℃, and insulation 2h; After reaction finished, room temperature to be naturally cooled to stopped logical nitrogen;

(4) product of step (3) is put into zero(ppm) water and soak, heated and boiled, washing, when pH=7, drying promptly obtains gac.

Described ionic liquid is [Bmim] PF ₆

Embodiment 3

(1) wooden or bamboo raw material are pulverized, screening filters out the raw material that particle size range is 0.5-2.5mm, puts into air dry oven, under 105 ℃, dries to constant weight;

(2) be the 10:1 thorough mixing by mass ratio at room temperature with the raw material and the ionic liquid of step (1), and dipping 2h;

(3) will be in the raw material after step (2) is handled be packed stainless steel tubular type reactor drum into, and be installed on the tube type resistance furnace, in stainless steel tubular type reactor drum, feed nitrogen then; Speed with 30 ℃/min is warming up to 400 ℃, and insulation 3h; Then the speed with 20 ℃/min is warming up to 900 ℃, and insulation 3h; After reaction finished, room temperature to be naturally cooled to stopped logical nitrogen;

(4) product of step (3) is put into zero(ppm) water and soak, heated and boiled, washing, when pH=7, drying promptly obtains gac.

Described ionic liquid is that volume ratio is [Bmim] PF of 10:1 ~ 10:3 ₆[Bmim] BF ₄Mixture.

Detection means:

1, iodine sorption value measuring method

Iodine sorption value according to GB/T 12496.7-90 detection of active charcoals.

A=

In the formula: the iodine sorption value of A-sample (mg/g);

c ₁The amount concentration (mol/L) of-iodine standard solution;

c ₂The amount concentration (mol/L) of-sodium thiosulfate standard solution;

v ₂The consumption of-hypo solution (mL);

M-sample mass (g);

The amount (g) of 127- iodine.

2, hole and specific area measuring method

Adopt the SSA4300 hole and the specific surface area analysis appearance of Beijing Bi Aode company to carry out N ₂Adsorption-desorption experiment, the preceding 200 ℃ of degassing 2 h of sample test, according to the specific surface area of BET Equation for Calculating gac ( A _BET), according to the pore size distribution of BJH formula calculated activity charcoal.

Fig. 1 is gac N under 77.4K ₂Adsorption isothermal line.Can know that by figure the charcoal absorption thermo-isopleth shows as I type (IUPAC classification), show that it is main with micropore; Adsorption equilibrium further shows the existence of atomic hole (Ultramicropore) in its structure in the just basic completion of very low relative pressure (less than 0.1).

Fig. 2 gac graph of pore diameter distribution has confirmed that further gac mainly is to think micropore and atomic Kong Weizhu, and the mesopore content of existence seldom.

The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.

Claims (3)

1. one kind is that acvator prepares process of active carbon with the ionic liquid, and it is characterized in that: wooden or bamboo raw material is the gac that acvator prepares high-specific surface area with the ionic liquid.

2. according to claim 1 is that acvator prepares process of active carbon with the ionic liquid, it is characterized in that: said method comprising the steps of:

(1) wooden or bamboo raw material are pulverized, screening filters out the raw material that particle size range is 0.5-2.5mm, puts into air dry oven, under 105 ℃, dries to constant weight;

(2) be 50:1 ~ 10:1 thorough mixing by mass ratio at room temperature, and flood 2 ~ 5h the raw material and the ionic liquid of step (1);

(3) will be in the raw material after step (2) is handled be packed stainless steel tubular type reactor drum into, and be installed on the tube type resistance furnace, in stainless steel tubular type reactor drum, feed nitrogen then; Speed with 10-30 ℃/min is warming up to 200-400 ℃, and insulation 0.5-3h; Then the speed with 5 ~ 20 ℃/min is warming up to 600-900 ℃, and insulation 1-3h; After reaction finished, room temperature to be naturally cooled to stopped logical nitrogen;

(4) product of step (3) is put into zero(ppm) water and soak, heated and boiled, washing, when pH=7, drying promptly obtains gac.

3. according to claim 2 is that acvator prepares process of active carbon with the ionic liquid, it is characterized in that: described ionic liquid is to contain in the ionic liquid of hexafluoro-phosphate radical or tetrafluoroborate one or several.

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