CN103408011A - Preparation method of sargassum horneri matrix activated carbon - Google Patents
Preparation method of sargassum horneri matrix activated carbon Download PDFInfo
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Abstract
The invention discloses a preparation method of sargassum horneri matrix activated carbon. The preparation method comprises the following steps: (1), mixing sargassum horneri powder and activator with water for impregnating treatment for 2-24 h; (2), placing the mixture I under an inert atmosphere, raising the temperature of the mixture I to 400-600 DEG C according to a rate of 10-30 DEG C/min; performing activating treatment on the mixture I for 1-3 h; then washing the mixture I with hot acid solution and hot distilled water in sequence until the pH value of the mixture does not change; drying the mixture I to obtain a product A; (3), mixing the product A with boiling oxidant solution to enable the product A to react with the boiling oxidant solution for 1-3 h; then, washing the mixture II with hot distilled water until the pH value of the mixture II does not change; drying the mixture II to obtain a product B; (4), performing high-heat treatment on the product B at 300-500 DEG C, so as to obtain the sargassum horneri matrix activated carbon. The activated carbon prepared through the preparation method has the advantages that most pores are mesoporous, the pores are well-developed, the ash content is low, and the adsorbability to hexavalent chromium is higher.
Description
Technical field
The present invention relates to a kind of preparation method of gac, characteristics are to take Sargassum horneri to prepare the method for gac as raw material.
Background technology
Gac is a kind of porous material, has flourishing pore texture, huge specific surface area, abundant surface functional group, the stable advantages such as chemical property, thereby is widely used.But the gac industry still belongs to " resource-hungry " industry at present substantially, thereby raw material sources are major reasons of restricted activity charcoal industry development.Raw material prepared by the gac of selecting both at home and abroad at present, mainly is divided into: coal, wooden and Industrial products and industrial and agricultural waste.In recent years, traditional raw material is subject to the restriction of the problems such as resource, the energy and environment, makes the sight of finding the gac raw material from land, turn to ocean gradually.Large quantity research shows, kelp has good heavy metal and the absorption property of organic pollutant, and often possess higher content of cellulose, and fast growth, output large, be easy to harvesting, with grain, do not strive the advantage such as ground, thereby have potentiality in the gac preparation field.In the world, since 2009, take two kinds of kelp Sargassum Longifolium (S.L.) and Hypnea Valentiae (H.V.) is raw material, by the proportioning of regulating the activator zinc chloride, control the gac pore size distribution, produce and take mesopore and be main gac, and the advantage that physical strength is high, ash oontent is low is arranged; Posidonia Oceanic (L.) fiber of take is raw material, adopts respectively steam activation method, zinc chloride activation method to carry out the preparation of gac.At present that kelp is less as the relevant report of gac raw materials, obtained gac specific surface area be take Sargassum horneri and is had no report as raw material but on the whole.
Gac is divided into charing and activation two steps usually, and traditional chemical activation method is large to equipment corrosion, residual in contaminate environment, gac the pharmaceutical chemicals activator arranged, and application facet is restricted.In carbonization process, most important factor is charing outlet temperature and charing heat-up rate, and the carbonizing production quality is also closely related with raw material chemical property and physics particle diameter etc.Activation temperature is to determine that activated carbon pore structure forms one of principal element of speed.The activation main reaction is reversible thermo-negative reaction, and the raising temperature of reaction is conducive to positive reaction carries out, but excess Temperature, the pore texture of gac easily changes, and micropore reduces, and macropore increases, strength degradation, yield reduces.Therefore, guarantee that yield, minimizing energy consumption, Optimization Technology, raising quality are the basic demand of Activated Carbon Production all the time.
Sargassum horneri (Sargassum Horneri) is the advantage species of China's southeastern coast, has been listed in first-selected species and one of important species of rebuilding submarine algae field that the warm extra large temperate zone marine eco-environment is repaired.But the industrialization of Sargassum horneri, recycling be ripe, urgently exploitation far away also.Therefore, utilize Sargassum horneri to prepare gac, become the advanced subject in Sargassum horneri Application and Development field.The research that the result of study of this patent gained can be the kelp matrix activated carbon provides basis and uses for reference, and also for the industrialized utilization of needing badly after the extensive non-consumption kelp of aquaculture in the marine ecology recovery project, carries out early-stage preparations simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of Sargassum horneri matrix activated carbon, and gac prepared by the method be take mesopore as main, and the hole prosperity, and ash oontent is low, and sexavalent chrome is had to higher absorption property.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of method for preparing gac with Sargassum horneri, comprise the steps:
(1) Sargassum horneri powder, activator and water are mixed, carry out dip treating 2～24h; Described activator is zinc chloride or phosphoric acid or potassium hydroxide; Wherein the weight ratio of Sargassum horneri powder and activator is 1:3～5;
(2) macerate is placed in to the speed by 10～30 ℃/min under inert atmosphere and is warming up to 400～600 ℃, carry out the activation treatment of 1～3h, then use the hot acid solution washing, the reusable heat distilled water wash is constant to pH, and drying obtains product A;
(3) product A is mixed with the oxidizing agent solution of boiling, reaction 1～3h, then wash the constant and dry product B that obtains to pH with hot distilled water;
(4) product B is carried out to high-temperature heat treatment 1～3h in 300～500 ℃, namely obtain Sargassum horneri matrix activated carbon product.
In the present invention, described Sargassum horneri powder can obtain by following processing: the fresh Sargassum horneri water that will gather cleans removes impurity, and cutting after drying, pulverize in pulverizer, and after preferably pulverizing, the particle diameter of Sargassum horneri powder is at 20～100 orders.
In described step (1), described activator is zinc chloride or phosphoric acid or potassium hydroxide, preferably zinc chloride or phosphoric acid, most preferably zinc chloride.Described dip treating is carried out under room temperature, stirring.The weight ratio of described Sargassum horneri powder and water is generally at 1:5.
In described step (2), described inert atmosphere is preferably nitrogen, and gas flow is 50～150L/h.The hydrochloric acid soln that the hot acid solution of washing use preferably boils.The temperature of the hot distilled water of washing use is generally at 70～100 ℃.
In described step (3), described oxygenant is nitric acid or sulfuric acid or the hydrochloric acid soln of 10～50% massfractions, preferably salpeter solution.In every 1g product A, the add-on of oxidizing agent solution is 5～20mL.The temperature of the hot distilled water of washing use is generally at 70～100 ℃.Described oxidizing reaction is at room temperature carried out.
In described step (2), (3), described drying is carried out respectively under the temperature condition of 100～110 ℃, and be 3～24h time of drying.
Sargassum horneri matrix activated carbon product prepared by the method for the invention, its specification is as follows: specific surface area 1014～2314m
2G
-1, iodine number 1005.7～1197.8mgg
-1, methylene blue value 9.0～12.0mL0.1g
-1, caramel percent of decolourization 90～115%, sexavalent chrome saturated extent of adsorption 24.2～83.5mgg
-1, ash oontent 0.2～0.8%.
Compared with prior art, beneficial effect of the present invention is:
(a) the present invention adopts the raw materials of Sargassum horneri as gac, and the oxygen level of Sargassum horneri is high, in carbonization process due to the fracture of oxygen-containing functional group, with H
2O, CO, CO
2The oxygen of emitting etc. form has further improved the reaming performance; Simultaneously because oxygen level is high, during thermolysis, easily and hydrogenation symphysis Cheng Shui, the tar generated or other plastic masss also will be relatively less.
(b) the present invention adopts the gac after chemical activation is further carried out to oxidation modification, high-temperature heat treatment, the activated carbon surface carboxyl, phenolic hydroxyl group, the acid oxygen-containing functional group content such as lactone group significantly improves, and find after pyroprocessing certain hour under felicity condition, can be in the situation that not disruptive oxidation functional group makes the blocked phenomenon in duct originally caused due to oxidation obtain better improvement, make the gac made and its compared with prior art have specific surface area high, the advantages such as the strong and ash oontent of specific absorption property is low, be specially adapted to the purification absorption of heavy metal ion-containing waste water, simultaneously, also can be for the adsorption cleaning process of other gas.
The accompanying drawing explanation
Fig. 1 is respectively the Sargassum horneri matrix activated carbon scanning electron microscope (SEM) photograph of example 1-4, and wherein A-embodiment 1, B-embodiment 2, C-embodiment 3, D-embodiment 4.
Embodiment
Below in conjunction with example, further describe technical characterstic of the present invention, but protection scope of the present invention is not limited to this.
Embodiment 1
To be collected in the Sargassum horneri in marine site, Zhe Nan Wenzhou, simple air-dryly with tap water, wash desalination, impurity afterwards, then with deionized water wash, drain for several times, under 100 ℃, dry 24h to constant weight.Dry Sargassum horneri is pulverized again, filters out 20～40 purpose powder.Take the dry Sargassum horneri powder of 10g, adding the 100g massfraction is 50% liquor zinci chloridi, stirs 2h under 25 ℃.Then dip compound is transferred in vacuum tube furnace, at flow 120Lh
-1Nitrogen protection under, with 10 ℃ of min
-1Speed be warming up to 500 ℃, the activation 1h.The sample 1molL that activation obtains
-1HCl solution boil 30min, continue with boiling the HCl solution washing for several times, constant to pH with the deionized water wash of 95 ℃ till, then baking 24h, to constant weight, obtains product A under 100 ℃
1.
To the 1g product A
1In add the boiling nitric acid solution of 10mL10%, 25 ℃ of standing oxidation 2h.Till the sample of oxidation is constant to pH with the deionized water wash of 95 ℃, then under 100 ℃, dry 24h to constant weight, obtain product B
1.By product B
1The retort furnace of putting into 300 ℃ carries out high-temperature heat treatment 2h, namely obtains activated carbon product C
1, its performance is in Table 1.
Embodiment 2
To be collected in the Sargassum horneri in marine site, Zhe Nan Wenzhou, simple air-dryly with tap water, wash desalination, impurity afterwards, then with deionized water wash, drain for several times, under 100 ℃, dry 24h to constant weight.Dry Sargassum horneri is pulverized again, filters out 20～40 purpose powder.Take the dry Sargassum horneri powder of 10g, adding the 100g massfraction is 50% liquor zinci chloridi, stirs 10h under 25 ℃.Then dip compound is transferred in vacuum tube furnace, at flow 100Lh
-1Nitrogen protection under, with 20 ℃ of min
-1Speed be warming up to 600 ℃, the activation 3h.The sample 1molL that activation obtains
-1HCl solution boil 30min, continue with boiling the HCl solution washing for several times, constant to pH with the deionized water wash of 95 ℃ till, then baking 24h, to constant weight, obtains product A under 100 ℃
2.
To the 1g product A
2In add the boiling nitric acid solution of 10mL20%, 25 ℃ of standing oxidation 1h.Till the sample of oxidation is constant to pH with the deionized water wash of 95 ℃, then under 100 ℃, dry 24h to constant weight, obtain product B
2.By product B
2The retort furnace of putting into 400 ℃ carries out high-temperature heat treatment 3h, namely obtains activated carbon product C
2, its performance is in Table 1.
Embodiment 3
To be collected in the Sargassum horneri in marine site, Zhe Nan Wenzhou, simple air-dryly with tap water, wash desalination, impurity afterwards, then with deionized water wash, drain for several times, under 100 ℃, dry 24h to constant weight.Dry Sargassum horneri is pulverized again, filters out 20～40 purpose powder.Take the dry Sargassum horneri powder of 10g, adding the 100g massfraction is 30% liquor zinci chloridi, stirs 10h under 25 ℃.Then dip compound is transferred in vacuum tube furnace, at flow 150Lh
-1Nitrogen protection under, with 30 ℃ of min
-1Speed be warming up to 600 ℃, the activation 1h.The sample 1molL that activation obtains
-1HCl solution boil 30min, continue with boiling the HCl solution washing for several times, constant to pH with the deionized water wash of 95 ℃ till, then baking 24h, to constant weight, obtains product A under 100 ℃
3.
To the 1g product A
3In add the boiling nitric acid solution of 10mL10%, 25 ℃ of standing oxidation 3h.Till the sample of oxidation is constant to pH with the deionized water wash of 95 ℃, then under 100 ℃, dry 24h to constant weight, obtain product B
3.By product B
3The retort furnace of putting into 500 ℃ carries out high-temperature heat treatment 2h, namely obtains activated carbon product C
3, its performance is in Table 1.
Embodiment 4
To be collected in the Sargassum horneri in marine site, Zhe Nan Wenzhou, simple air-dryly with tap water, wash desalination, impurity afterwards, then with deionized water wash, drain for several times, under 100 ℃, dry 24h to constant weight.Dry Sargassum horneri is pulverized again, filters out 20～40 purpose powder.Take the dry Sargassum horneri powder of 10g, adding the 100g massfraction is 50% phosphoric acid solution, stirs 10h under 25 ℃.Then dip compound is transferred in vacuum tube furnace, at flow 100Lh
-1Nitrogen protection under, with 10 ℃ of min
-1Speed be warming up to 400 ℃, the activation 1h.The sample 1molL that activation obtains
-1HCl solution boil 30min, continue with boiling the HCl solution washing for several times, constant to pH with the deionized water wash of 95 ℃ till, then baking 24h, to constant weight, obtains product A under 100 ℃
4.
To the 1g product A
4In add the boiling nitric acid solution of 10mL30%, 25 ℃ of standing oxidation 2h.Till the sample of oxidation is constant to pH with the deionized water wash of 95 ℃, then under 100 ℃, dry 24h to constant weight, obtain product B
4.By product B
4The retort furnace of putting into 400 ℃ carries out high-temperature heat treatment 1h, namely obtains activated carbon product C
4, its performance is in Table 1.
Embodiment 5
To be collected in the Sargassum horneri in marine site, Zhe Nan Wenzhou, simple air-dryly with tap water, wash desalination, impurity afterwards, then with deionized water wash, drain for several times, under 100 ℃, dry 24h to constant weight.Dry Sargassum horneri is pulverized again, filters out 20～40 purpose powder.Take the dry Sargassum horneri powder of 10g, adding the 100g massfraction is 30% phosphoric acid solution, stirs 10h under 25 ℃.Then dip compound is transferred in vacuum tube furnace, at flow 100Lh
-1Nitrogen protection under, with 20 ℃ of min
-1Speed be warming up to 400 ℃, the activation 2h.The sample 1molL that activation obtains
-1HCl solution boil 30min, continue with boiling the HCl solution washing for several times, constant to pH with the deionized water wash of 95 ℃ till, then baking 24h, to constant weight, obtains product A under 100 ℃
5.
To the 1g product A
5In add the boiling nitric acid solution of 10mL20%, 25 ℃ of standing oxidation 3h.Till the sample of oxidation is constant to pH with the deionized water wash of 95 ℃, then under 100 ℃, dry 24h to constant weight, obtain product B
5.By product B
5The retort furnace of putting into 300 ℃ carries out high-temperature heat treatment 2h, namely obtains activated carbon product C
5, its performance is in Table 1.
The test of Sargassum horneri matrix activated carbon structure properties:
Adopt the U.S. ASAP2020 of Micromeritics company automatic absorbing instrument to measure the specific surface area of gac, its specific surface area is calculated by standard BET method.Adopt surface topography and the pore texture of the Japanese Hitachi HitachiS-4700 of company sem observation gac.
The mensuration of ash of active carbon content is carried out with reference to " GB/T12496.3-1999 " wood activated charcoal ash content test method; The mensuration of iodine sorption value is carried out with reference to " GB/T12496.8-1999 " wood activated charcoal iodine sorption value measuring method; The mensuration of caramel percent of decolourization is carried out with reference to " GB/T12496.9-1999 " wood activated charcoal caramel percent of decolourization measuring method; The adsorptive value of methylene blue is measured with reference to " GB/T12496.10-1999 " wood activated charcoal iodine sorption value measuring method and is carried out; Cr
6+The mensuration of concentration adopts adjacent dinitrodiphenyl carbazide development process, calculates Cr according to Law of Lambert-Beer
6+Concentration, and the loading capacity of calculated activity charcoal.
Table 1 Sargassum horneri matrix activated carbon performance
Claims (8)
1. the preparation method of a Sargassum horneri matrix activated carbon, comprise the steps:
(1) Sargassum horneri powder, activator and water are mixed, carry out dip treating 2～24h; Described activator is zinc chloride or phosphoric acid or potassium hydroxide; Wherein the weight ratio of Sargassum horneri powder and activator is 1:3～5;
(2) macerate is placed in to the speed by 10～30 ℃/min under inert atmosphere and is warming up to 400～600 ℃, carry out the activation treatment of 1～3h, then use the hot acid solution washing, the reusable heat distilled water wash is constant to pH, and drying obtains product A;
(3) product A is mixed with the oxidizing agent solution of boiling, reaction 1～3h, then wash the constant and dry product B that obtains to pH with hot distilled water;
(4) product B is carried out to high-temperature heat treatment 1～3h in 300～500 ℃, namely obtain Sargassum horneri matrix activated carbon product.
2. according to preparation method claimed in claim 1, it is characterized in that: the median size of the Sargassum horneri powder described in step (1) is 20～100 orders.
3. according to preparation method claimed in claim 1, it is characterized in that: the activator described in step (1) is zinc chloride or phosphoric acid.
4. according to preparation method claimed in claim 1, it is characterized in that: the inert atmosphere described in step (2) is nitrogen.
5. according to preparation method claimed in claim 1, it is characterized in that: the oxidizing agent solution described in step (3) is nitric acid or sulfuric acid or the hydrochloric acid soln of 10～50% massfractions.
6. according to preparation method claimed in claim 1, it is characterized in that: the oxidizing agent solution described in step (3) is the salpeter solution of 10～50% massfractions.
7. according to the described preparation method of claim 1 or 5, it is characterized in that: in step (3), in every 1g product A, the add-on of oxidizing agent solution is 5～20mL.
8. according to preparation method claimed in claim 1, it is characterized in that: the drying in step (2), (3) is carried out respectively under the temperature condition of 100～110 ℃, and be 3～24h time of drying.
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| CN109261137A (en) * | 2018-09-30 | 2019-01-25 | 江苏斯沃得环保科技有限公司 | A kind of composite reactive Carbon Materials and preparation method |
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| CN108298535A (en) * | 2018-03-15 | 2018-07-20 | 浙江工业大学 | A kind of continuous production method of Sargassum horneri mesopore activated carbon |
| CN109261137A (en) * | 2018-09-30 | 2019-01-25 | 江苏斯沃得环保科技有限公司 | A kind of composite reactive Carbon Materials and preparation method |
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Effective date of registration: 20221212 Address after: 037000 Xi Han Ling Xiang Bei Cun Nan Cun, Yungang District, Datong City, Shanxi Province Patentee after: Datong Jinsheng Haoda Carbon Industry Co.,Ltd. Address before: 11th floor, donglecheng international, Shuguang Road, Chengguan Street, Dongming County, Heze City, Shandong Province Patentee before: Heze Jianshu Intelligent Technology Co.,Ltd. |
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