CN102211767A - Granular activated carbon prepared from xanthoceras sorbifolia bunge aril and process thereof - Google Patents
Granular activated carbon prepared from xanthoceras sorbifolia bunge aril and process thereof Download PDFInfo
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Abstract
The invention discloses granular activated carbon prepared from xanthoceras sorbifolia bunge aril and a process thereof. The process comprises the following steps: (1) smashing the xanthoceras sorbifolia bunge aril, drying and then smashing after pretreatment (namely sieving); (2) carrying out acid leaching; (3) drying and activating; and (4) rinsing, drying and sieving so as to obtain the finished activated carbon. The method has the advantages that the xanthoceras sorbifolia bunge aril as a raw material for preparing the activated carbon is abundant, and the raw material is from processing residues of xanthoceras sorbifolia biodiesel so that waste is turned into wealth; based on the xanthoceras sorbifolia bunge aril as the raw material, and the activated carbon is prepared by a phosphoric acid solution activation process, thus the preparation process is simple, the production cost is reduced, the pollution is less, and the activated carbon is easy to regenerate and is good in chemical stability; and the activated carbon prepared by the phosphoric acid solution activation process has the advantages of large specific surface area and good absorption property.
Description
Technical field:
The present invention relates to a kind of gac and processing method, especially relate to and a kind ofly prepare granulated active carbon and processing method with the shinyleaf yellowhorn fruit shell.
Background technology:
Absorption is to separate and a kind of important technology of scavenging process, and in many sorbing materials, gac has obtained application the most widely because of its big adsorptive power and cheap cost.Be widely used in fields such as chemical industry, environmental protection, food and pharmacy, support of the catalyst and electrode materials.Inner Mongolia Autonomous Region is residuums such as the main product area of Wood of Shinyleaf Yellowhorn, processing and utilization shinyleaf yellowhorn fruit shell, and it is turned waste into wealth, to the comprehensive utilization of Wood of Shinyleaf Yellowhorn with build a conservation-minded society and have great importance.
Wood of Shinyleaf Yellowhorn (Xanthoceras sorbifolia Bunge) is the woody oleiferous plants crop that the Sapindaceae Wood of Shinyleaf Yellowhorn belongs to, be China's endemic tree, originate in the northern China loess plateau, wild, have characteristics such as drought resisting, cold-resistant, barren-resistant, salt tolerant alkali, counting provinces and regions in northern China has artificial growth, is mainly used in and checks winds and fixes drifting sand.China's ancient book herbal for Relief of Famines record: Wood of Shinyleaf Yellowhorn kind benevolence is distinguished the flavor of sweet edible.Wood of Shinyleaf Yellowhorn kind benevolence oil-containing is rich in 14 kinds of unsaturated fatty acidss more than 60% in the oil, be the edible oil that has good quality, the dregs of fat after the oil expression contain rich in protein, be high-quality feed, the Wood of Shinyleaf Yellowhorn seed kernel oil also can be used as technical oils and medicinal, also is the high quality raw material of production biofuel.And the shinyleaf yellowhorn fruit shell accounts for more than 30% of Wood of Shinyleaf Yellowhorn seed weight, so rationally utilizes shinyleaf yellowhorn fruit shell resource, to improve its using value.Yet up to now, the thing that shinyleaf yellowhorn fruit shell etc. are discarded is not exploited as yet.
Summary of the invention:
The object of the present invention is to provide a kind of have raw material extensively, pollute less, easily regeneration, production cost is low, chemical stability good, absorption property well can large-scale production power prepares the processing method of granulated active carbon with the shinyleaf yellowhorn fruit shell.
Second purpose of the present invention is to provide a kind of granulated active carbon with the preparation of shinyleaf yellowhorn fruit shell by method for preparing.
First purpose of the present invention is implemented by following technical scheme: the processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell; it includes following steps: the Wood of Shinyleaf Yellowhorn seed hulls is pulverized; dry after the pre-treatment of sieving; with phosphoric acid solution with after the pre-treatment and exsiccant Wood of Shinyleaf Yellowhorn seed hulls crushed material carry out acidleach; carry out charing, activation then; the rinsing drying and screening is refining to be the black powder gac then, gets product.
Prepare the preferred method of the technology of granulated active carbon with the shinyleaf yellowhorn fruit shell, it includes following steps:
(1) the Wood of Shinyleaf Yellowhorn seed hulls is pulverized drying, crushing screening again after the pre-treatment of sieving, choose 20-60 purpose particle, get Wood of Shinyleaf Yellowhorn seed hulls crushed material, put drying in the constant temperature electric heating loft drier, Wood of Shinyleaf Yellowhorn seed hulls crushed material moisture content is reduced to below 10%; Pretreated shinyleaf yellowhorn fruit shell particle is put into pulverizer further pulverize,, choose 60-120 purpose shinyleaf yellowhorn fruit shell particle shinyleaf yellowhorn fruit shell grinding and sieving;
(2) acidleach: get the phosphoric acid solution that mass percent concentration is 60%-90%, with Wood of Shinyleaf Yellowhorn seed hulls crushed material in the step (1) and the mass percent concentration for preparing is that the phosphoric acid solution of 60%-90% stirs repeatedly and rubs pressure, make and mix, the solid-to-liquid ratio that wherein said Wood of Shinyleaf Yellowhorn seed hulls crushed material and the described mass percent concentration for preparing are the phosphoric acid solution of 60%-90% is 1.5 by mass volume ratio: 1--2.5: 1;
(3) charing, activation: the Wood of Shinyleaf Yellowhorn seed hulls after the acidleach is heating charing 10-12h in 200-230 ℃ of following loft drier earlier; Putting into resistance furnace then heightens temperature to 400 ℃--and 500 ℃, enter activation stage, the soak time of Wood of Shinyleaf Yellowhorn seed hulls gac is controlled at 90-150min;
(4) rinsing, drying, sieve finished product: gac is taken out, add the clear water repetitive scrubbing, making pH value is 5-7; The gac that will wet is put in the 100-120 ℃ of loft drier dry, and the water ratio of gac is reduced to below 10%, and pulverizes, and obtains finished product shinyleaf yellowhorn fruit shell granular active carbon after sieving, in the sealing bag of packing into.
Drying requires constant temperature in loft drier in described step (1), and temperature is 90-110 ℃.
Second purpose of the present invention implemented by following technical scheme: a kind of prepared shinyleaf yellowhorn fruit shell granular active carbon of processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell.
The invention has the advantages that: prepare gac raw material abundance with the shinyleaf yellowhorn fruit shell, raw material turns waste into wealth it from the industrial wood waste of Wood of Shinyleaf Yellowhorn biofuel; With the shinyleaf yellowhorn fruit shell is raw material, and it is simple that the phosphoric acid solution activating process prepares active charcoal preparing process, and production cost reduces, pollutes less, the charcoal activation temperature is low; It is big that phosphoric acid activation method prepares shinyleaf yellowhorn fruit shell gac specific surface area, and absorption property is good.
Description of drawings:
Fig. 1 is the preparation technology figure of shinyleaf yellowhorn fruit shell gac of the present invention.
Fig. 2 is the methylene blue percent of decolourization comparison diagram of embodiment of the invention 1-3 shinyleaf yellowhorn fruit shell gac.
Fig. 3 is a magenta adsorptive capacity of the present invention graphic representation over time.
Fig. 4 is the shinyleaf yellowhorn fruit shell gac iodine number adsorptive capacity comparison diagram of embodiment of the invention 1-3.
Specific embodiments:
Embodiment 1: as shown in Figure 1; a kind of processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell is made up of following steps: (1) pulverizes the Wood of Shinyleaf Yellowhorn seed hulls; dry after the pre-treatment of sieving; crushing screening again; choose 20 purpose particles, get Wood of Shinyleaf Yellowhorn seed hulls crushed material, put in the constant temperature electric heating loft drier dry; drying requires constant temperature in loft drier, and temperature is 90 ℃.Wood of Shinyleaf Yellowhorn seed hulls crushed material moisture content is reduced to below 10%; Pretreated shinyleaf yellowhorn fruit shell particle is put into pulverizer further pulverize,, choose 60 purpose shinyleaf yellowhorn fruit shell particles shinyleaf yellowhorn fruit shell grinding and sieving;
(2) acidleach: get mass percent concentration and be 60% phosphoric acid solution, with Wood of Shinyleaf Yellowhorn seed hulls crushed material in the step (1) and the mass percent concentration for preparing is that 60% phosphoric acid solution stirs repeatedly and rubs pressure, make to mix, quicken the infiltration of phosphoric acid solution to shinyleaf yellowhorn fruit shell inside.Wherein said Wood of Shinyleaf Yellowhorn seed hulls crushed material and the described mass percent concentration for preparing are 60% phosphoric acid solution by the solid-to-liquid ratio mass volume ratio is to mix stirring at 1.5: 1.
(3) charing, activation: the Wood of Shinyleaf Yellowhorn seed hulls after the acidleach is heating charing 10h in 200 ℃ of following loft drier earlier; Put into resistance furnace then temperature is heightened to 400 ℃, enter activation stage, the soak time of Wood of Shinyleaf Yellowhorn seed hulls gac is controlled at 90min;
(4) rinsing, drying, sieve finished product: gac is taken out, add the clear water repetitive scrubbing, making the pH value is 5; The gac that will wet is put in 100 ℃ of loft drier dry, and the water ratio of gac is reduced to below 10%, and pulverizes, and obtains finished product shinyleaf yellowhorn fruit shell granular active carbon after sieving, in the sealing bag of packing into.
Embodiment 2: as shown in Figure 1; a kind of processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell is made up of following steps: (1) pulverizes the Wood of Shinyleaf Yellowhorn seed hulls; dry after the pre-treatment of sieving; crushing screening again; choose 60 purpose particles, get Wood of Shinyleaf Yellowhorn seed hulls crushed material, put in the constant temperature electric heating loft drier dry; drying requires constant temperature in loft drier, and temperature is 110 ℃.Wood of Shinyleaf Yellowhorn seed hulls crushed material moisture content is reduced to below 10%; Pretreated shinyleaf yellowhorn fruit shell particle is put into pulverizer further pulverize,, choose 120 purpose shinyleaf yellowhorn fruit shell particles shinyleaf yellowhorn fruit shell grinding and sieving;
(2) acidleach: get mass percent concentration and be 90% phosphoric acid solution, with Wood of Shinyleaf Yellowhorn seed hulls crushed material in the step (1) and the mass percent concentration for preparing is that 90% phosphoric acid solution stirs repeatedly and rubs pressure, make to mix, quicken the infiltration of phosphoric acid solution to shinyleaf yellowhorn fruit shell inside.Wherein said Wood of Shinyleaf Yellowhorn seed hulls crushed material and the described mass percent concentration for preparing be 90% phosphoric acid solution be 2.5: 1 mixing and stirring by the solid-to-liquid ratio mass volume ratio.
(3) charing, activation: the Wood of Shinyleaf Yellowhorn seed hulls after the acidleach is heating charing 12h in 230 ℃ of following loft drier earlier; Put into resistance furnace then temperature is heightened to 500 ℃, enter activation stage, the soak time of Wood of Shinyleaf Yellowhorn seed hulls gac is controlled at 150min;
(4) rinsing, drying, sieve finished product: gac is taken out, add the clear water repetitive scrubbing, making the pH value is 7; The gac that will wet is put in 120 ℃ of loft drier dry, and the water ratio of gac is reduced to below 10%, and pulverizes, and obtains finished product shinyleaf yellowhorn fruit shell granular active carbon after sieving, in the sealing bag of packing into.
Embodiment 3: as shown in Figure 1; a kind of processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell is made up of following steps: (1) pulverizes the Wood of Shinyleaf Yellowhorn seed hulls; dry after the pre-treatment of sieving; crushing screening again; choose 40 purpose particles, get Wood of Shinyleaf Yellowhorn seed hulls crushed material, put in the constant temperature electric heating loft drier dry; drying requires constant temperature in loft drier, and temperature is 100 ℃.Wood of Shinyleaf Yellowhorn seed hulls crushed material moisture content is reduced to below 10%; Pretreated shinyleaf yellowhorn fruit shell particle is put into pulverizer further pulverize,, choose 90 purpose shinyleaf yellowhorn fruit shell particles shinyleaf yellowhorn fruit shell grinding and sieving;
(2) acidleach: get mass percent concentration and be 75% phosphoric acid solution, with Wood of Shinyleaf Yellowhorn seed hulls crushed material in the step (1) and the mass percent concentration for preparing is that 75% phosphoric acid solution stirs repeatedly and rubs pressure, make to mix, quicken the infiltration of phosphoric acid solution to shinyleaf yellowhorn fruit shell inside.Wherein said Wood of Shinyleaf Yellowhorn seed hulls crushed material and the described mass percent concentration for preparing are that 75% phosphoric acid solution is 2.0: 1 mixing and stirring by the solid-to-liquid ratio mass volume ratio.
(3) charing, activation: the Wood of Shinyleaf Yellowhorn seed hulls after the acidleach is heating charing 11h in 210 ℃ of following loft drier earlier; Put into resistance furnace then temperature is heightened to 450 ℃, enter activation stage, the soak time of Wood of Shinyleaf Yellowhorn seed hulls gac is controlled at 120min;
(4) rinsing, drying, sieve finished product: gac is taken out, add the clear water repetitive scrubbing, making the pH value is 6; The gac that will wet is put in 110 ℃ of loft drier dry, and the water ratio of gac is reduced to below 10%, and pulverizes, and obtains finished product shinyleaf yellowhorn fruit shell granular active carbon after sieving, in the sealing bag of packing into.
Experimental example 4: by the prepared gac of the invention described above embodiment, the gac of gained carries out methylene blue percent of decolourization, magenta adsorptive capacity and three evaluation indexes of iodine number, weighs the performance of the shinyleaf yellowhorn fruit shell gac of phosphoric acid method preparation.
4.1 methylene blue percent of decolourization
The methylene blue solution 20mL that accurate absorption concentration is 5mg/L puts and is heated to 90 ℃ on the electric furnace in the 250mL Erlenmeyer flask.Accurately take by weighing shinyleaf yellowhorn fruit shell gac 0.02g with analytical balance, embodiment 1,2 and 3 prepared gacs are poured into respectively in the Erlenmeyer flask, take off behind the stirring 20min.With the cooling of the solution in the Erlenmeyer flask, get supernatant liquor on spectrophotometer, measure 670nm place absorbancy with the ICM cuvette.Be calculated as follows percent of decolourization then.
Method of calculation are: percent of decolourization (%)=(A
0-A)/A
0* 100%
A
0-the absorbancy of methylene blue solution before handling
Methylene blue solution absorbancy after A-handles
At maximum absorption wavelength is that to record concentration be 5mg/L methylene blue solution absorbance A at the 670nm place
0Be 0.7447, methylene blue solution is decoloured, and calculate percent of decolourization, as shown in Figure 2.
4.2 magenta adsorptive capacity
The Basic Fuchsin in Aqueous Solution of preparation 300mg/l adds respectively in the 0.04g shinyleaf yellowhorn fruit shell gac that embodiment 1,2 and 3 weighs up successively, puts into constant temperature oscillator every 5 minutes and vibrates, and temperature is set at 30 ℃, measures the magenta adsorptive capacity.Shinyleaf yellowhorn fruit shell gac is more stable to the adsorptive capacity change curve of magenta as shown in Figure 3, increases along with the prolongation of time, and the interior at one time rising with temperature increases.When surpassing 30min, the adsorptive capacity of shinyleaf yellowhorn fruit shell charcoal absorption magenta tends towards stability, press gac that embodiment 2 methods prepare to the adsorptive capacity of magenta apparently higher than other enforcement groups, high adsorption capacity 344.9348mg/g.
4.3 iodine number
The shinyleaf yellowhorn fruit shell gac 0.1000g that accurately takes by weighing embodiment 1,2 and 3 preparations is in Erlenmeyer flask, put into exsiccant 100mL iodine flask, accurately adding people's (1+9 drips) hydrochloric acid 10.0mL makes sample moistening, be placed on to be heated on the electric furnace and boil, little 30s that boils, after being cooled to room temperature, add the 0.1mol/L iodine standard solution of people 50.0mL.Filled in bottle cap immediately, the 15min that vibrates on vibrating machine is filled into rapidly in the dry beaker.With pipette, extract 10.0mL filtrate, put in the people 250mL iodine flask, add 100mL water, carry out titration with the 0.1mol/L sodium thiosulfate standard solution, when solution is faint yellow, add the 2mL Starch Indicator, it is colourless that the continuation titration becomes solution, notes the Sulfothiorine volume (as shown in Figure 4) of use.Be calculated as follows iodine number:
Method of calculation: iodine number E=5 (10C
1-V * C
2) * 126.9/m
C in the formula
1Be iodine solution concentration, V is a titration milliliter number, C
2Be the concentration of Sulfothiorine, m is for accurately taking by weighing the gram number of gac.The concentration of iodine liquid is measured by the 0.1mol/L sodium thiosulfate standard solution.1278.46mg/g。
Can learn that by evaluation index the shinyleaf yellowhorn fruit shell gac of embodiment 2 methods preparation has good methylene blue percent of decolourization and reaches 96.05%; Adsorptive capacity to magenta is up to 344.9438mg/g; The adsorptive capacity of iodine number is 1278.46mg/g, all meets the iodine number standard of country-level gac, is higher than methylene blue percent of decolourization, magenta adsorptive capacity and the iodine number adsorptive capacity of common gac.
Claims (4)
1. the processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell; it includes following steps: the Wood of Shinyleaf Yellowhorn seed hulls is pulverized; the pre-treatment of sieving is dry afterwards; with phosphoric acid solution with after the pre-treatment and exsiccant Wood of Shinyleaf Yellowhorn seed hulls crushed material carry out acidleach; carry out charing, activation then; the rinsing drying and screening is refining to be the black powder gac then, gets product.
2. according to claim 1ly a kind ofly prepare the processing method of granulated active carbon with the shinyleaf yellowhorn fruit shell, it includes following steps:
(1) the Wood of Shinyleaf Yellowhorn seed hulls is pulverized drying, crushing screening again after the pre-treatment of sieving, choose 20-60 purpose particle, get Wood of Shinyleaf Yellowhorn seed hulls crushed material, put drying in the constant temperature electric heating loft drier, Wood of Shinyleaf Yellowhorn seed hulls crushed material moisture content is reduced to below 10%; Pretreated shinyleaf yellowhorn fruit shell particle is put into pulverizer further pulverize,, choose 60-120 purpose shinyleaf yellowhorn fruit shell particle shinyleaf yellowhorn fruit shell grinding and sieving;
(2) acidleach: get the phosphoric acid solution that mass percent concentration is 60%-90%, with Wood of Shinyleaf Yellowhorn seed hulls crushed material in the step (1) and the mass percent concentration for preparing is that the phosphoric acid solution of 60%-90% is 1.5 by the solid-to-liquid ratio mass volume ratio: 1--2.5: 1 mixes, and stirs repeatedly to make to evenly;
(3) charing, activation: the Wood of Shinyleaf Yellowhorn seed hulls after the acidleach heats charing 10-12h earlier down in 200-230 ℃ of loft drier; Putting into resistance furnace then heightens temperature to 400 ℃--and-500 ℃, enter activation stage, the soak time of Wood of Shinyleaf Yellowhorn seed hulls gac is controlled at 90-150min;
(4) rinsing, drying, sieve finished product: gac is taken out, add the clear water repetitive scrubbing, making pH value is 5-7; The gac that will wet is put in the 100-120 ℃ of loft drier dry, and the water ratio of gac is reduced to below 10%, and pulverizes, and obtains finished product shinyleaf yellowhorn fruit shell granular active carbon after sieving, and gets product.
3. according to claim 2ly a kind ofly prepare the processing method of granulated active carbon with the shinyleaf yellowhorn fruit shell, drying requires constant temperature in loft drier in described step (1), and temperature is 90-110 ℃.
4. according to the arbitrary described a kind of prepared shinyleaf yellowhorn fruit shell granular active carbon of processing method for preparing granulated active carbon with the shinyleaf yellowhorn fruit shell of claim 1-3.
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| CN110227421A (en) * | 2019-06-18 | 2019-09-13 | 内蒙古农业大学 | A kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel |
| CN111302339A (en) * | 2020-02-24 | 2020-06-19 | 山东大学 | Porous carbon material prepared from xanthoceras sorbifolia bunge shell residue waste as well as preparation method and application of porous carbon material |
| CN112017871A (en) * | 2020-08-31 | 2020-12-01 | 深圳职业技术学院 | Composite electrode material and preparation method and application thereof |
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