CN103011160A - Method for preparing active carbon by utilizing tamarix chinensis - Google Patents
Method for preparing active carbon by utilizing tamarix chinensis Download PDFInfo
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- CN103011160A CN103011160A CN2012105852598A CN201210585259A CN103011160A CN 103011160 A CN103011160 A CN 103011160A CN 2012105852598 A CN2012105852598 A CN 2012105852598A CN 201210585259 A CN201210585259 A CN 201210585259A CN 103011160 A CN103011160 A CN 103011160A
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Abstract
The invention relates to a method for preparing active carbon by utilizing tamarix chinensis. The method comprises the following steps of: cutting branches of the tamarix chinensis; airing or drying and pulverizing the branches to prepare tamarix chinensis powder; adding phosphoric acid with the concentration of 50-60 percent by weight into the tamarix chinensis powder to soak for 12-18 hours in a mixing mode according to the mass ratio of the tamarix chinensis powder and the phosphoric acid of (1:2)-(1:3); heating the soaked tamarix chinensis powder at 100 DEG C and rising the temperature to 300 DEG C to ensure that the temperature rising velocity is 4-6 DEG C/minutes; continuously heating the tamarix chinensis powder to 400-600 DEG C to keep the temperature for 4-5 hours; cooling the tamarix chinensis powder to be at constant temperature to prepare an active carbon intermediate product; soaking the active carbon intermediate product with diluted hydrochloric acid or hot water for 30-40 minutes; washing the product by distilled water until a pH value is 5-7 after soaking; drying at 80-110 DEG C; and grinding and pulverizing the product to prepare active carbon. By the method, the production source of active carbon raw materials is widened, the production cost of the active carbon is reduced, an iodine sorption value of the produced active carbon can be up to 1,100mg/g, and the yield is high.
Description
Technical field
The present invention relates to a kind of preparation method of gac, concrete is a kind of method of utilizing Chinese tamarisk to prepare gac, belongs to the gac preparing technical field.
Background technology
Gac is a kind of high-quality sorbent material, have unique pore texture and surfactivity functional group, have enough chemical stabilities, physical strength and acidproof, alkaline-resisting, heat-resisting, and water insoluble and organic solvent, use the superperformances such as the rear easily regeneration of losing efficacy, at aspects such as food-processing, pharmacy, chemistry, metallurgy, agricultural, environmental protection extremely extensive and important application is arranged, it is too high directly to adopt timber (such as rapid-result poplar etc.) to do the cost that starting material need, and is not suitable for producing gac.In recent years, coal and wood chip shortage of resources were on the rise, and new processing condition, the increase new variety of raw material, exploration of therefore continually developing Activated Carbon Production are vital tasks of China and even World Activated Carbon industrial development.Problem for traditional gac raw materials shortage of resources, developed in recent years and utilized shell, sawdust, cereal shell, Pericarppium arachidis hypogaeae, rice straw to prepare gac for raw material, obtained preferably achievement, but adopt the discarded plant tissue such as shell, sawdust, cereal shell, Pericarppium arachidis hypogaeae to prepare gac, starting material are collected difficulty on the one hand, the raw material of preparation gac is subject to great restriction, is difficult to realize scale of mass production.Another is convenient because the formation gac mainly relies on the organic xylogen in the starting material, Mierocrystalline cellulose etc., and xylogen in the discarded plant tissue such as above-mentioned shell, sawdust, cereal shell, Pericarppium arachidis hypogaeae, content of cellulose are few, and raw-material difference causes the charcoal absorption spread in performance for preparing uneven.
Chinese patent CN102211767 discloses a kind of shinyleaf yellowhorn fruit shell and has prepared granulated active carbon and processing method, comprises the steps: that (1) pulverize the shinyleaf yellowhorn fruit shell, sieve process after drying pulverize again (2) acidleach, (3) dry, activation; (4) rinsing, drying, the finished product gac that sieves to get, raw material turns waste into wealth it from the industrial wood waste of Wood of Shinyleaf Yellowhorn biofuel, and technique is simple, and it is low to manufacture a finished product.But there is following shortcoming in this patent: 1, Wood of Shinyleaf Yellowhorn has a very limited distribution, fraction of coverage is lower, 2, the Wood of Shinyleaf Yellowhorn fruit-setting rate is subjected to environmental influence larger, causes its fruit-setting rate fluctuation larger, and this two aspects factor causes the shinyleaf yellowhorn fruit husk as raw material to be limited by very large.If it is improper that 3 kinds are selected, after setting and grow up, Wood of Shinyleaf Yellowhorn can form fruitless " thousand the spend a fruit " phenomenon of only blooming, and this target that not only can not reach high yield creation economic benefit has also wasted the resources such as soil and labor force.
Chinese tamarisk is temperate zone and tropical trees, and distribution area is wide, and vitality is extremely strong, and happiness light, drought-enduring, cold-resistant is also more water-fast wet.Utmost point Salt And Alkali Tolerance, sandy bare land, well developed root system, germinating power is strong, and extremely anti-pruning cradles.Delta Region of The Yellow River is that Chinese tamarisk is in the main range of distribution of China.Because Huanghe delta degree of salinity is higher, other plant is difficult to growth, and the Huanghe delta Chinese tamarisk of special Salt And Alkali Tolerance is the On behalf of plant of this regional vegetation, and it has almost spread all over each corner in this piece soil.The Chinese tamarisk branch of pruning often is dropped, burns or rots, and not only environment is exerted a certain influence, and has also wasted resource.
Summary of the invention
For prior art gac scarcity of raw material, and the low deficiency of Chinese tamarisk branch utilization ratio the invention provides a kind of method of utilizing Chinese tamarisk to prepare gac.The present invention adopts Huanghe delta Chinese tamarisk branch as raw material, and abundant raw material is easy to get, and has enlarged the raw-material source of production gac, reduces the cost of producing gac.
The raw material explanation:
The Chinese tamarisk branch that the present invention adopts is taken from the Huanghe delta, and wherein moisture accounts for 4.9～5.4wt%, ash content 2.2～2.6wt%, and organic 92.0～92.9wt%, organic matter is mainly xylogen and wood fibre.
Technical scheme of the present invention is as follows:
A kind of method of utilizing Chinese tamarisk to prepare gac comprises the steps:
(1) gets the Chinese tamarisk branch, dry after the cutting or dry, pulverize, cross 20～40 mesh sieves, make the Chinese tamarisk powder;
(2) the Chinese tamarisk powder of getting under the sieve adds the phosphoric acid mixing immersion that concentration is 50～60wt%, and described Chinese tamarisk powder is 1:2～1:3 with the phosphoric acid quality ratio, and described soak time is 12～18 hours;
(3) the Chinese tamarisk powder after step (2) is soaked is heated to 300 ℃ by 100 ℃, and described temperature rise rate is 4～6 ℃/min; Continue heating, being heated to temperature is 400 ℃～600 ℃, is incubated 4～5 hours, is cooled to normal temperature, makes the gac intermediate product;
(4) get the gac intermediate product that step (3) makes, with dilute hydrochloric acid or hot-water soak 30～40 minutes, being washed to the pH value with distilled water again after the immersion was 5～7, then dried under 80～110 ℃ of conditions, ground, pulverized, and made gac.
The present invention is preferred, and the described temperature of drying of step (1) is 20 ℃～30 ℃, and bake out temperature is 100 ℃～110 ℃.
The present invention is preferred, and soaking conditions is in the step (2): soaked 12 hours under the normal temperature, the concentration of phosphoric acid is 50wt%, and the Chinese tamarisk powder is 1:3 with the phosphoric acid quality ratio.
The present invention is preferred, heating in the step (3) is that the Chinese tamarisk powder after step (2) is soaked joins in the crucible, place retort furnace to heat in crucible again, temperature is heated to 300 ℃ by 100 ℃ in the described retort furnace, described temperature rise rate is 5 ℃/min, continuation is heated retort furnace, and being heated to temperature is 400 ℃, soaking time 4～5 hours.
The present invention is preferred, and the dilute hydrochloric acid in the step (4) is the dilute hydrochloric acid of concentration 1wt%～5wt%, and the temperature of hot water is 60 ℃～80 ℃.With dilute hydrochloric acid or the favourable impurity of removing in the gac intermediate product of hot-water soak, immersion is fully dissolved impurity.
This employing Chinese tamarisk branch is that raw material prepares gac, utilizes phosphoric acid to activate Chinese tamarisk and has changed raw-material pyrolytic process.About 200 ℃, basically finished the charing stage, form stable polycondensation carbon structure at 200～300 ℃, 300～600 ℃ of roomy temperature ranges, the charcoal body is corroded in selectively slow oxidation of phosphoric acid in the presence of oxygen, can think the main temperature range of activation, especially about 400 ℃, can prepare the high-quality measured gac of yield, after 600 ℃, the effusion of gasifying gradually of phosphoric acid carbon structure with certain fire-resistant oxidation resistant ability, the charcoal material loses the protection of phosphoric acid and is burnt and lose; The whole pyrolytic process of the present invention all is in the state without exothermic effect, and the gac porosity of preparing is high, and iodine sorption value can reach 1100mg/g.
Advantage of the present invention is as follows:
1, the preparation method of gac of the present invention does not have particular requirement to the kind of Chinese tamarisk, can utilize the Chinese tamarisk resource of China's abundant as starting material, thereby enlarged the raw-material source of production gac, and can reduce the cost of producing gac, the activated carbon-iodine adsorptive value of production can reach 1100mg/g.
2, at Delta Region of The Yellow River, Chinese tamarisk is as the representative plant in saltings, and is extremely strong in the adaptability in habitat, the Huanghe delta, and it is vigorous to grow, and biomass is large, and widely distribution is also arranged throughout the country.Utilize the Chinese tamarisk branch to produce gac as starting material, take full advantage of on the one hand resource, to this policy of response State Council's " Huanghe delta high eco-economy district development program ", be significant on the other hand.
3, to adopt Chinese tamarisk to prepare the yield of gac higher in the present invention.Adopt at present the more yield of producing gac take Pericarppium arachidis hypogaeae as starting material to be 20%～30%, the yield that the present invention adopts Chinese tamarisk to prepare gac can reach 40%～48.5%.
Description of drawings
Fig. 1-Fig. 2 is the stereoscan photograph of the different enlargement ratios of the gac that makes of embodiment 1,
Fig. 3-Fig. 4 is the stereoscan photograph of the different enlargement ratios of the gac that makes of embodiment 2,
Embodiment
The present invention will be further described below in conjunction with embodiment.Per-cent among the embodiment all is weight percentage.The pulverizer that uses among the embodiment adopts all flag arrow Q-250A3 pulverizers of Electrical Appliances Co., Ltd of upper sea ice.
Embodiment 1
Get the cutting of 100g Chinese tamarisk branch, 100 ℃ of lower oven dry, pulverize with pulverizer, cross 20 mesh sieves, get the Chinese tamarisk powder 20g under the sieve, take by weighing the phosphatase 24 0g of concentration 50wt%, both are put into the beaker mixing and stirring and placed 12 hours, Chinese tamarisk powder after the immersion moves in the crucible with cover, place retort furnace to heat in crucible again, temperature is heated to 300 ℃ by 100 ℃ in the retort furnace, and described temperature rise rate is 5 ℃/min, continues retort furnace is heated, being heated to temperature is 400 ℃, is incubated 5 hours.Stopped heating is cooled to behind the normal temperature crucible is taken out, and makes the gac intermediate product; To make the gac intermediate product and put into beaker, and add the dilute hydrochloric acid 40ml of 1wt%, soak 30 minutes, being washed with distilled water to pH value is 6 again, puts into loft drier with 90 ℃ of oven dry of constant temperature 6 hours, obtains gac 9.7g.
The gac electromicroscopic photograph of gained as shown in Figure 1, 2, by Fig. 1-Fig. 2 as can be known, the activation of prepared gac fully, micropore is flourishing, specific surface area is large.
Test charcoal absorption experiment:
The gac that present embodiment makes is measured iodine sorption value by method shown in the GB/T12496.8-1999, and iodine sorption value is 1100mg/g; Measure methylene blue adsorption value by method that GB/T12496.10-1999 releases, methylene blue adsorption value is 15ml/0.1g.
Embodiment 2
Get the cutting of 100g Chinese tamarisk branch, 100 ℃ of lower oven dry, pulverize with pulverizer, cross 20 mesh sieves, get the Chinese tamarisk powder 20g under the sieve, take by weighing the phosphoric acid 60g of concentration 50wt%, both are put into the beaker mixing and stirring and placed 12 hours, Chinese tamarisk powder after the immersion moves in the crucible with cover, place retort furnace to heat in crucible again, temperature is heated to 300 ℃ by 100 ℃ in the retort furnace, and described temperature rise rate is 4 ℃/min, continues retort furnace is heated, being heated to temperature is 550 ℃, soaking time 4 hours.Stopped heating is cooled to behind the normal temperature crucible is taken out, and makes the gac intermediate product; To make the gac intermediate product and put into beaker, and add 75 ℃ hot water, soak 30 minutes, being washed with distilled water to PH is 6 again, puts into loft drier with 90 ℃ of oven dry of constant temperature 6 hours, takes out and obtains gac 9.4g.
The gac electromicroscopic photograph of gained is shown in Fig. 3,4, and by Fig. 3-Fig. 4 as can be known, prepared gac activation is complete, and micropore is flourishing, and specific surface area is large.
Test charcoal absorption experiment:
The gac that present embodiment makes is measured iodine sorption value by method shown in the GB/T12496.8-1999, and iodine sorption value is 1040mg/g; Measure methylene blue adsorption value by method that GB/T12496.10-1999 releases, methylene blue adsorption value is 11ml/0.1g.
The contrast experiment:
Comparative Examples 1:
Preparation method's step of gac as described in Example 1, difference is: preparation gac employed raw material is Pericarppium arachidis hypogaeae, and prepared gac is used for contrast experiment's comparative analysis.
Comparative Examples 2:
Preparation method's step of gac as described in Example 1, difference is: preparation gac employed raw material is the millet shell, and prepared gac is used for contrast experiment's comparative analysis.
Chemical method prepares the concept that gac generally adopts yield, i.e. the ratio of product quality and raw materials quality, and its calculating formula is:
Yield (%)=m product/m raw material * 100%,
Iodine sorption value is measured: presses GB/T12496.8-1999 and measures iodine sorption value,
Methylene blue adsorption value is measured: method that GB/T12496.10-1999 releases is measured methylene blue adsorption value.
The gac that adopts different materials to make above-mentioned Comparative Examples 1, Comparative Examples 2, the gac that yield, iodine sorption value and methylene blue adsorption value and the embodiment 1 of the gac that makes adopts the Chinese tamarisk branch to make is made a simultaneous test table, the raw material that adopts is different, and corresponding yield, iodine sorption value and methylene blue adsorption value contrast effect are listed in (referring to table 1) in the table 1
Table 1
| Project | Yield | Iodine sorption value | Methylene blue adsorption value |
| Embodiment 1 | 48.5% | 1100mg/g | 15ml/0.1g |
| Comparative Examples 1 | 38% | 950mg/g | 13ml/0.1g |
| Comparative Examples 2 | 35% | 800mg/g | 11ml/0.1g |
As seen result by 3 groups of experiment gained in the upper table 1 contrasts, under same preparation condition, employing Chinese tamarisk of the present invention prepares the yield of gac greater than adopting Pericarppium arachidis hypogaeae, millet shell to prepare the yield of gac, experiment shows, under the equal conditions, the employing amount of raw material is identical, adopts Chinese tamarisk to prepare output that gac obtains greater than adopting Pericarppium arachidis hypogaeae, millet shell to prepare the output of gac.From the gac that makes to the adsorptive value of iodine, methylene blue to recently, the employing Chinese tamarisk prepares the iodine sorption value of gac, prepares the iodine sorption value of gac greater than employing Pericarppium arachidis hypogaeae, millet shell, the employing Chinese tamarisk prepares the methylene blue adsorption value of gac, prepares the methylene blue adsorption value of gac greater than employing Pericarppium arachidis hypogaeae, millet shell, thereby can find out that the absorption property of the gac of Chinese tamarisk preparation is better than adopting the absorption property of the gac of Pericarppium arachidis hypogaeae, the preparation of millet shell.
Economic cost analysis: estimate through the data that the sky, Shandong of interview collection on the spot source activity charcoal company limited provides, the activated carbon product explant price of iodine number more than 800mg/g is 5-6 ten thousand/ton at present, its material cost is about 1.7 ten thousand, human cost is about 1.8 ten thousand, remove the more relevant little incidentals such as other transportations, profit is considerable again.Because Chinese tamarisk is produced activated carbon product iodine number absorption and reaches 1000mg/g in the experiment, belongs to high grade activated carbon, therefore can apply production.
Claims (5)
1. a method of utilizing Chinese tamarisk to prepare gac comprises the steps:
(1) gets the Chinese tamarisk branch, dry after the cutting or dry, pulverize, cross 20～40 mesh sieves, make the Chinese tamarisk powder;
(2) the Chinese tamarisk powder of getting under the sieve adds the phosphoric acid mixing immersion that concentration is 50～60wt%, and described Chinese tamarisk powder is 1:2～1:3 with the phosphoric acid quality ratio, and described soak time is 12～18 hours;
(3) the Chinese tamarisk powder after step (2) is soaked is heated to 300 ℃ by 100 ℃, and described temperature rise rate is 4～6 ℃/min; Continue heating, being heated to temperature is 400 ℃～600 ℃, is incubated 4～5 hours, is cooled to normal temperature, makes the gac intermediate product;
(4) get the gac intermediate product that step (3) makes, with dilute hydrochloric acid or hot-water soak 30～40 minutes, being washed to the pH value with distilled water again after the immersion was 5～7, then dried under 80～110 ℃ of conditions, ground, pulverized, and made gac.
2. the method for utilizing Chinese tamarisk to prepare gac according to claim 1 is characterized in that, the described temperature of drying of step (1) is 20 ℃～30 ℃, and bake out temperature is 100 ℃～110 ℃.
3. the method for utilizing Chinese tamarisk to prepare gac according to claim 1 is characterized in that, soaking conditions is in the step (2): soaked 12 hours under the normal temperature, the concentration of phosphoric acid is 50wt%, and the Chinese tamarisk powder is 1:3 with the phosphoric acid quality ratio.
4. arbitrary described method of utilizing Chinese tamarisk to prepare gac according to claim 1-3, it is characterized in that, heating in the step (3) is that the Chinese tamarisk powder after step (2) is soaked joins in the crucible, place retort furnace to heat in crucible again, temperature is heated to 300 ℃ by 100 ℃ in the described retort furnace, and described temperature rise rate is 5 ℃/min, continues retort furnace is heated, being heated to temperature is 400 ℃, soaking time 4～5 hours.
5. the method for utilizing Chinese tamarisk to prepare gac according to claim 1 is characterized in that, the dilute hydrochloric acid in the step (4) is the dilute hydrochloric acid of concentration 1wt%～5wt%, and the temperature of hot water is 60 ℃～80 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771413A (en) * | 2014-01-02 | 2014-05-07 | 福建农林大学 | Method for preparing active carbon by organic sodium activator |
| CN103910359A (en) * | 2014-01-24 | 2014-07-09 | 内蒙古农业大学 | Method for preparing active carbon from shinyleaf yellowhorn wood biodiesel processing residue |
| CN106140100A (en) * | 2015-05-14 | 2016-11-23 | 厦门大学嘉庚学院 | A kind of methylene blue method of wastewater treatment |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774833A (en) * | 2011-05-10 | 2012-11-14 | 西北农林科技大学 | Method of preparing active carbon from cork wood |
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2012
- 2012-12-30 CN CN2012105852598A patent/CN103011160A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774833A (en) * | 2011-05-10 | 2012-11-14 | 西北农林科技大学 | Method of preparing active carbon from cork wood |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103771413A (en) * | 2014-01-02 | 2014-05-07 | 福建农林大学 | Method for preparing active carbon by organic sodium activator |
| CN103771413B (en) * | 2014-01-02 | 2015-12-09 | 福建农林大学 | The method of gac prepared by a kind of organic sodium activator |
| CN103910359A (en) * | 2014-01-24 | 2014-07-09 | 内蒙古农业大学 | Method for preparing active carbon from shinyleaf yellowhorn wood biodiesel processing residue |
| CN106140100A (en) * | 2015-05-14 | 2016-11-23 | 厦门大学嘉庚学院 | A kind of methylene blue method of wastewater treatment |
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Application publication date: 20130403 |