CN102633259A - Preparation method for jute-based active carbon - Google Patents
Preparation method for jute-based active carbon Download PDFInfo
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Abstract
The invention discloses a preparation method for jute-based active carbon, and the method comprises the following steps of: weighing jute fibres or crushed jute stem materials, cleaning and drying, soaking in a beaker filled with a 3-5mol/L phosphoric acid solution, boiling for 3-10 hours in a water bath, adequately penetrating an activating agent into the fibres, then taking out and drying; placing in a vacuum tubular high-temperature sintering furnace, activating to 400-500 DEG C in a nitrogen atmosphere, insulating for 1-3 hours, or placing in a columnar quartz tube, placing in a microwave device, and performing a microwave irradiation reaction with a microwave irradiation power of 100-700 W and an irradiation time of 5-30 minutes in the presence of nitrogen used as protective gas; and cooling to a room temperature, then taking out, acid-washing and repeatedly water-washing until the pH is 6-7, and then drying to obtain the jute-based active carbon. The jute-based active carbon prepared by the method has the advantage of being high in methylene blue adsorption value and activation yield.
Description
Technical field
The present invention relates to a kind of preparation method of jute matrix activated carbon, belong to the manufacturing technology field of gac.
Background technology
Gac is a kind of carbonaceous sorbing material that enriches pore texture and huge specific surface area that has; Have characteristics such as high adsorption capacity, mechanical strength is high, chemicalstability is good, can conveniently regenerate, be widely used in fields such as industry, agricultural, traffic, medical and health, national defence, environment protection.Along with the raising day by day of environmental protection requirement, the demand of gac is the trend that rises year by year both at home and abroad in recent years.
The raw material of tradition Preparation of Activated Carbon mainly is timber and coal.Because domestic forest tree resource is limited and reduce day by day, coal price is higher, seek cheapness and abundant renewable raw materials substitutes timber and coal is present Preparation of Activated Carbon field urgent problem.In recent years, be the research focus that the feedstock production gac becomes gac development of raw materials aspect gradually with cotton stalk, rice husk, stalk, corn cob, Pericarppium arachidis hypogaeae, corn straw, coconut husk, nut-shell equal yield line agricultural wastes big and cheap and easy to get.
Fibre of flax for textile material makes the gac of preparation have unique physics, chemisorption performance because of having special construction and chemical ingredients, and therefore the research with various fibre of flax for textile material feedstock production gacs such as Chinese fiber crops, sisal hemp, ramies also receives much concern.Corchorus phloem fiber crop for Tiliaceae annual herb plant, mainly is made up of Mierocrystalline cellulose, semicellulose and xylogen, in addition, also contains a small amount of pectin, wax etc.China is one of area of origin of jute, and cultivation history is long, and variety source is abundant; Be the third-largest in the world jute producing country, cultivated area is about 1,000 ten thousand mu, and YO is at 1,100,000 tons; The major production areas is on the south the Changjiang river, and is bigger with Zhejiang, Guangdong, Taiwan San Sheng cultivated area.Mainly be to utilize tossa to make commodity such as the rope made of hemp, gunnysack, linen in the industry, numb strain centre portions (being commonly called as " waste of flax ") remaining behind the jute degumming causes the significant wastage and the environmental pollution of resource then by a large amount of discarded or burnings.Because tossa has the structure of hollow, and content of lignin is all higher in tossa and the jute bar, thereby be the quality matetrial of preparation gac.
From preparation method of active carbon, the mode that general selection is heated raw material, common type of heating is electric furnace heating method and microwave heating method.But, traditional electric furnace type of heating consumption worker, consuming time, power consumption, and material is heated irregular.Microwave heating technique then is through the to-and-fro movement of heated object internal dipole molecule high frequency; Produce " internal friction heat " and make and be heated the material temperature and raise; Do not need any heat transfer process just can make material inside and outside portion heat simultaneously, heat up simultaneously; Rate of heating is fast and evenly, required time is merely the part of traditional heating mode, even 1/tens.In addition, because of microwave heating does not need that the body of heater heating is not had additional heat consumption, can improve energy utilization rate to greatest extent.
Therefore, utilize microwave radiation tossa or jute bar to prepare gac, not only can reduce soak time, save energy, and can turn waste into wealth, improve farmers' income." the microwave radiation potassium hydroxide method prepares jute bar activated carbon process " (Zhu Yanli etc., Yunnan chemical, the 32nd the 3rd phase of volume of June in 2005) discloses a kind of microwave radiation potassium hydroxide method and prepared jute bar activated carbon process; The jute bar is broken, oven dry are immersed in the certain density potassium hydroxide solution, in UW, make its dispersing and mixing 1h; Then 120 ℃ down behind the dehydration 5h in microwave oven heat-activated; Activated material is through pickling, rinsing, dry gac.Show that through experiment the alkali carbon ratio is 1, soak time is 14 minutes, and microwave power is 700 watt-hours, and making the activated carbon iodine sorption value is 1264.02mg/g, and methylene blue adsorption value is 210mg/g, yield of activation 11.29%.Because the kenaf stalk activated charcoal methylene blue adsorption value of this prepared is merely 210mg/g, therefore poor to the adsorptive power and the decoloring ability of pigment, yield of activation is merely 11.29% in addition, causes jute bar wastage of material, and economic benefit is low.Therefore need to improve technology, select better to be more suitable for the chemical activating agent of jute bar, and parameters such as the concentration of chemical activating agent, activation temperature, soak time, kenaf stalk activated charcoal methylene blue adsorption value and yield of activation improved.
Summary of the invention
Technical problem to be solved by this invention is the low and low problem of yield of activation of kenaf stalk activated charcoal methylene blue adsorption value for preparing in the prior art, and the preparation method of the high jute based activated carbon of a kind of methylene blue adsorption value height and yield of activation is provided.
A kind of preparation method of jute matrix activated carbon, it may further comprise the steps:
(1) pre-treatment: take by weighing tossa or pulverize after the oven dry of jute bar raw material for washing, uses concentration to flood as the chemical activating agent of 3-5 mol/L, 3-10h is boiled in water-bath, then with its taking-up, oven dry;
(2) charing-activation: will place activation furnace through the raw material that step (1) is handled, charing and activation in nitrogen atmosphere, activation temperature is 400-500 ℃, soak time is 1-3 hour; Perhaps in microwave device be that protection gas carries out charing and activation with nitrogen, microwave exposure power is 100-700W, and irradiation time is 5-30min;
(3) aftertreatment: will dry after being 6-7 through pickling, repeated water washing to pH value with its taking-up after tossa that step (2) is handled or jute bar are cooled to room temperature, promptly get the jute matrix activated carbon.
Said chemical activating agent is any one or more in phosphoric acid solution, liquor zinci chloridi, sodium hydroxide solution, the ammonium dibasic phosphate solution.
Said chemical activating agent is a phosphoric acid, and concentration is 4mol/L.
Said activation temperature is 450 ℃, and soak time is 1 hour.
Said activation temperature is 450 ℃, and soak time is 2 hours.
Said activation temperature is 400 ℃, and soak time is 2 hours.
Said microwave exposure power is 500W, and irradiation time is 10min.
Said microwave exposure power is 400W, and irradiation time is 15min.
Said microwave exposure power is 600W, and irradiation time is 10min.
Said microwave exposure power is 700W, and irradiation time is 5min.
The present invention has following advantage:
The present invention utilizes tossa and jute bar to make the added value that gac not only can improve the jute industrial chain, can also save valuable timber and coal resources, has important economic benefit and environmental benefit.Select the chemical activating agent of proper concn for use, water-bath is boiled, and makes the abundant infiltrated fiber of acvator inner; Under nitrogen protection,, select proper temperature and soak time through cremator activation or microwave exposure activation; Gained gac yield is about 40%, and the about 300mg/g of methylene blue adsorption value is all far above the jute bar gac of prior art with the preparation of microwave radiation potassium hydroxide method; Improved the utilization ratio of tossa and jute bar, the gained gac is strong to the adsorptive power and the decoloring ability of pigment.
Embodiment
Embodiment 1
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 3mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the activation furnace, in nitrogen atmosphere, activation temperature is 400 ℃ again, and soak time is 1 hour, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 45.02%, and iodine sorption value is 878.62mg/g, the about 299.7mg/g of methylene blue adsorption value.
Embodiment 2
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 3mol/L, 3h is boiled in water-bath, then with its taking-up, oven dry; Put it into the electron tubes type high temperature sintering furnace again, in nitrogen atmosphere, activation temperature is 450 ℃, and soak time is 2 hours, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 41.88%, and iodine sorption value is 1079.9mg/g, the about 299.23mg/g of methylene blue adsorption value.
Embodiment 3
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 4mol/L, 4h is boiled in water-bath, then with its taking-up, oven dry; Put it into the electron tubes type high temperature sintering furnace again, in nitrogen atmosphere, activation temperature is 450 ℃, and soak time is 1 hour, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 43.67%, and iodine sorption value is 1221.13mg/g, the about 360.14mg/g of methylene blue adsorption value.
Embodiment 4
Take by weighing the jute bar after 10 g pulverize, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 5mol/L, 3h is boiled in water-bath, then with its taking-up, oven dry; Put it in the activation furnace, in nitrogen atmosphere, activation temperature is 450 ℃ again, and soak time is 1 hour, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.26%, and iodine sorption value is 1125.51mg/g, the about 299.82mg/g of methylene blue adsorption value.
Embodiment 5
Take by weighing the jute bar after 10 g pulverize, clean oven dry, immerse and be equipped with in the beaker of liquor zinci chloridi that 0.2L concentration is 4mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it into the electron tubes type high temperature sintering furnace again, in nitrogen atmosphere, activation temperature is 450 ℃, and soak time is 1 hour, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.38%, and iodine sorption value is 1108.51mg/g, the about 296.42mg/g of methylene blue adsorption value.
Embodiment 6
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of sodium hydroxide solution that 0.2L concentration is 4mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it into the electron tubes type high temperature sintering furnace again, in nitrogen atmosphere, activation temperature is 450 ℃, and soak time is 1 hour, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 41.25%, and iodine sorption value is 1028.51mg/g, the about 286.42mg/g of methylene blue adsorption value.
Embodiment 7
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of ammonium dibasic phosphate solution that 0.2L concentration is 4mol/L, 6h is boiled in water-bath, then with its taking-up, oven dry; Put it into the electron tubes type high temperature sintering furnace again, in nitrogen atmosphere, activation temperature is 450 ℃, and soak time is 1 hour, is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.25%, and iodine sorption value is 1048.36mg/g, the about 296.62mg/g of methylene blue adsorption value.
Embodiment 8
Take by weighing the jute bar after 10g pulverizes, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 4mol/L, 4h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 300W, microwave exposure 30min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 41.57%, and iodine sorption value is 1021.13mg/g, the about 334.16mg/g of methylene blue adsorption value.
Embodiment 9
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 4mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 500W, microwave exposure 15min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.37%, and iodine sorption value is 1018.15mg/g, the about 323.15mg/g of methylene blue adsorption value.
Embodiment 10
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 5mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 400W, microwave exposure 20min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.57%, and iodine sorption value is 1013.25mg/g, the about 327.25mg/g of methylene blue adsorption value.
Embodiment 11
Take by weighing the jute bar after 10g pulverizes, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 4mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 600W, microwave exposure 10min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.08%, and iodine sorption value is 1015.32mg/g, the about 319.27mg/g of methylene blue adsorption value.
Embodiment 12
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of phosphoric acid solution that 0.2L concentration is 4mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 700W, microwave exposure 5min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 39.27%, and iodine sorption value is 1013.12mg/g, the about 313.17mg/g of methylene blue adsorption value.
Embodiment 13
Take by weighing the jute bar after 10g pulverizes, clean oven dry, immerse and be equipped with in the beaker of liquor zinci chloridi that 0.2L concentration is 3mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 400W, microwave exposure 15min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.17%, and iodine sorption value is 1019.32mg/g, the about 321.18mg/g of methylene blue adsorption value.
Embodiment 14
Take by weighing the 10g tossa, clean oven dry, immerse and be equipped with in the beaker of sodium hydroxide solution that 0.2L concentration is 4mol/L, 5h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 500W, microwave exposure 15min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 41.07%, and iodine sorption value is 1031.12mg/g, the about 318.12mg/g of methylene blue adsorption value.
Embodiment 15
Take by weighing the jute bar after 10g pulverizes, clean oven dry, immerse and be equipped with in the beaker of ammonium dibasic phosphate solution that 0.2L concentration is 4mol/L, 4h is boiled in water-bath, then with its taking-up, oven dry; Put it in the column silica tube again, place microwave device, set microwave power 500W, microwave exposure 15min under nitrogen protection is cooled to after the room temperature its taking-up, dries after PH is 6-7 through pickling, repeated water washing, promptly gets the jute matrix activated carbon.Wherein the gac yield is 40.47%, and iodine sorption value is 1061.02mg/g, the about 315.32mg/g of methylene blue adsorption value.
Analysis of experimental data
Jute based activated carbon preparation technology gac yield of the present invention is minimum to be 39.27%, is up to 45.02%, be documents gac yield 11.29% 3.47-3.98 doubly.Methylene blue adsorption value is minimum to be 286.42mg/g, is up to 360.14mg/g, is 1.36-1.74 times of documents methylene blue adsorption value 210mg/g.
Though the present invention has carried out detailed elaboration through above-mentioned specific embodiment to it; But; Any form that does not exceed the claim protection domain that those skilled in the art should be understood that on this basis to be made and the variation of details all belong to invention which is intended to be protected.
Claims (10)
1. the preparation method of a jute matrix activated carbon, it may further comprise the steps:
(1) pre-treatment: take by weighing tossa or pulverize after the oven dry of jute bar raw material for washing, uses concentration to flood as the chemical activating agent of 3-5 mol/L, 3-10h is boiled in water-bath, then with its taking-up, oven dry;
(2) charing-activation: will place activation furnace through the raw material that step (1) is handled, charing and activation in nitrogen atmosphere, activation temperature is 400-500 ℃, soak time is 1-3 hour; Perhaps in microwave device be that protection gas carries out charing and activation with nitrogen, microwave exposure power is 100-700W, and irradiation time is 5-30min;
(3) aftertreatment: will dry after being 6-7 through pickling, repeated water washing to pH value with its taking-up after tossa that step (2) is handled or jute bar are cooled to room temperature, promptly get the jute matrix activated carbon.
2. the preparation method of jute matrix activated carbon according to claim 1 is characterized in that: said chemical activating agent is any one or more in phosphoric acid solution, liquor zinci chloridi, sodium hydroxide solution, the ammonium dibasic phosphate solution.
3. the preparation method of jute matrix activated carbon according to claim 2 is characterized in that: said chemical activating agent is a phosphoric acid, and concentration is 4mol/L.
4. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said activation temperature is 450 ℃, and soak time is 1 hour.
5. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said activation temperature is 450 ℃, and soak time is 2 hours.
6. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said activation temperature is 400 ℃, and soak time is 2 hours.
7. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said microwave exposure power is 500W, and irradiation time is 10min.
8. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said microwave exposure power is 400W, and irradiation time is 15min.
9. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said microwave exposure power is 600W, and irradiation time is 10min.
10. according to the preparation method of claim 2 or 3 described jute matrix activated carbons, it is characterized in that: said microwave exposure power is 700W, and irradiation time is 5min.
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| CN103553037A (en) * | 2013-09-25 | 2014-02-05 | 蚌埠德美过滤技术有限公司 | Jute stalk modified active carbon and preparation method thereof |
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| CN103173894B (en) * | 2013-03-28 | 2014-08-20 | 西北工业大学 | Preparation method for repairing defects by converting hemp fibers into carbon fibers |
| CN103173894A (en) * | 2013-03-28 | 2013-06-26 | 西北工业大学 | Preparation method for repairing defects by converting hemp fibers into carbon fibers |
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Application publication date: 20120815 |