CN106362685A - Modified biochar material for removing arsenic, and preparation and application thereof - Google Patents
Modified biochar material for removing arsenic, and preparation and application thereof Download PDFInfo
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- CN106362685A CN106362685A CN201610822736.6A CN201610822736A CN106362685A CN 106362685 A CN106362685 A CN 106362685A CN 201610822736 A CN201610822736 A CN 201610822736A CN 106362685 A CN106362685 A CN 106362685A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention relates to a modified biochar material for removing arsenic, and preparation and application thereof. The preparation method comprises the following steps: adding biomass raw material powder into an ultrasonically-dispersed suspension of red mud and water, stirring the suspension to mix uniformly, and performing solid-liquid separation; roasting a obtained mixture of biomass and the red mud in a non-oxidizing atmosphere at the roasting temperature of 550 to 650 DEG C to obtain a carbonized product, namely, the modified biochar material. The modified biochar material is wide in raw material source, is convenient to prepare, has relatively high adsorption performance for arsenic-containing wastewater, is easy for large-scale production, and has a good application prospect.
Description
Technical field
The present invention relates to arsenic pollution treatment technology is and in particular to a kind of modification biological Carbon Materials for arsenic removal, its preparation
And application.
Background technology
Arsenic (as) is the metalloid element of a kind of " carcinogenic ", has important impact to human health.In recent years, portion of China
Region-by-region water body arsenic pollution event and arseniasiss phenomenon are appeared in the newspapers repeatly.Both domestic and external at present go dearsenicating method mainly to have: absorption, from
Sub- exchange, electric flocculation, film process, reverse osmosiss and bioanalysises etc..Wherein, absorption method is current comparative maturity, simple, application
Widely process the arsenic pollution technology of water environment.Absorption method is that specific surface area is big, loose structure solid material by using having
Material fixes arsenic in water body pollutant using mechanism of action such as physical absorption, chemisorbed and ion exchanges.
Red mud is the high alkalinity garbage producing in aluminum oxide industry production process.Global red mud adds up storage capacity and is up to
36.5 hundred million tons, and with annual 1.2 hundred million tons of speed increase.Therefore, suitable red mud disposal options are explored, effectively utilizes red mud provides
Source has become one of urgent task that domestic and international aluminum oxide industry faces.Domestic at present adsorb the grinding of arsenic in water using red mud
Study carefully.
Charcoal is that under conditions of anoxia or anoxybiotic, pyrolytic carbon burns and obtains using straw the like waste, has larger ratio
Surface area, distribution of pores are flourishing, the characteristic of stable chemical nature, and it is applied in soil not only can also improve carbon fixation and emission reduction
Soil, improves the yield of crops, is deeply favored by numerous scholars in recent years, is used for administering water body arsenic as a kind of adsorbent
Pollution.Chinese patent application (publication No. cn 104971697a) discloses a kind of magnetic bio charcoal removing arsenic in water body pollution
The preparation of material, has higher clearance to arsenic-containing waste water, and non-secondary pollution.But this invention with nano magnetite is
One of raw material, relatively costly, preparation process is more complicated, is unfavorable for large-area popularization and application.Chinese patent application (publication No. cn
104815613a) disclose a kind of preparation method and applications carrying lanthanum charcoal arsenic-removing adsorption agent, for processing in waste water body
Pentavalent arsenic ion, but the cost intensive of rare-earth elements of lanthanum, are not suitable for actual utilization and extention.
Content of the invention
It is an object of the invention to provide the good modification biological Carbon Materials for arsenic removal of a kind of low cost, absorption property, its
Preparation and application.
The technical scheme is that a kind of preparation method of the modification biological Carbon Materials for arsenic removal, comprising:
Biomass material powder is added in red mud through ultrasonic disperse and the suspension of water, stirring and evenly mixing and then solid-liquid
Separate；
The roasting under nonoxidizing atmosphere by the biomass obtaining and red mud mixture, 550～650 DEG C of sintering temperature, obtain
Carbonizing production, as modification biological Carbon Materials.
In a specific embodiment, described biomass material is rice straw.
In a specific embodiment, red mud and distilled water solid-to-liquid ratio 1:200～300g/ in the suspension of red mud and water
Ml, biomass material powder and red mud mass ratio are 3～7:1.
In a specific embodiment, ul-trasonic irradiation 30min～2h is obtained the suspension of red mud and water.
In a specific embodiment, described stirring and evenly mixing is, stirs 2～4h, then standing separation.
In a specific embodiment, the carbonized product deionized water drip washing obtaining removes impurity, using 1mol/l
agno3Solution whether there is cl to detect in leacheate-, and leacheate is neutrality.
In a specific embodiment, it is warming up to 550～650 DEG C with the heating rate of 4～6 DEG C/min during roasting, then
Insulation 5～8h.
The present invention also provides a kind of modification biological Carbon Materials for arsenic removal obtaining using above-mentioned preparation method.Bet method
The specific surface area measuring is 180～190m2/ g, has red mud granule in the area load of charcoal, and mineral composition contains fe2o3、
fe3o4、caco3、feo(oh)、al(oh)3And catio3.Its xrd collection of illustrative plates is as shown in the rm-bc of accompanying drawing 3.
The present invention also provides a kind of application of the described modification biological Carbon Materials for arsenic removal, for arsenic-containing water body arsenic removal,
Adjust water body ph during absorption as (v) 2～6, adsorb and adjust water body ph during as (iii) 8～12.
The red mud base charcoal of the present invention, fully combines charcoal (specific surface area is larger) and red mud (containing substantial amounts of ferrum
Aluminum oxide and oh group) advantage, have stronger absorption and co-precipitation to arsenate or arsenite ion.(sub-)
Arsenate can carry out ligand exchange with fixative surface hydroxyl, forms monodentate or bidentate monokaryon coordination sphere complex.
The present invention has the advantage that
1. the main production raw material of the red mud base biological carbon materials of the present invention is that process for making alumina trade waste is red
The biomass such as mud and agricultural wastes rice straw, raw material sources are wide, and low cost is it is achieved that the utilization of resources and turning waste into wealth.
2. red mud base charcoal of the present invention has higher removal effect to arsenic in water body, and experiment proves that solid-to-liquid ratio is 1:250
(g/ml), when, under optimum conditions 5923ug g is up to 10mg/l pentavalent arsenic ion adsorption capacity-1, to 10mg/l trivalent arsenic
Ion adsorption capacity is 520.0ug g-1.
3. the preparation process is simple of red mud base biological carbon materials of the present invention, production operation is convenient, beneficial to large-scale application.
Extensively, preparation is convenient, and has higher absorption property to arsenic-containing waste water for raw material sources of the present invention, easily carries out big
The production of scale, application prospect is good.Recycling for red mud and straw are turned waste into wealth one new approaches of offer simultaneously, tool
There is the benefit of higher economic, social and environment.
The red mud modification biological charcoal of the present invention is applied to the arsenic removal operation of arsenic polluted water body, can using manually adding,
Machinery sprays or other modes.
Brief description
Fig. 1 is the sem comparison diagram of the material of the embodiment of the present invention 1 preparation, and in figure a, b, c, d are represented as unmodified life respectively
Thing charcoal, red mud base charcoal, red mud base charcoal adsorb as (v) and adsorb the pattern after as (iii) with red mud base charcoal afterwards；
Fig. 2 is the eds comparison diagram of the material of the embodiment of the present invention 1 preparation, and in figure upper left, upper right, lower-left and bottom-right graph are divided
Do not represent unmodified charcoal, red mud base charcoal, red mud base charcoal absorption as (v) afterwards, red mud base charcoal absorption as
(iii) collection of illustrative plates after；
Fig. 3 is the xrd contrast of the unmodified charcoal (bc) of the embodiment of the present invention 1 preparation, red mud base charcoal (rm-bc)
Figure；
Fig. 4 is that in the embodiment of the present invention 2, ph adsorbs to as (v) and as (iii) to unmodified charcoal, red mud base charcoal
The impact comparison diagram of performance, wherein a, b are respectively shown in right to unmodified charcoal (bc), red mud base charcoal (rm-bc) for ph
The impact of as (v) absorption property, ph is to unmodified charcoal (bc), red mud base charcoal (rm-bc) to as (iii) absorption property
Impact；
Fig. 5 is unmodified charcoal in the embodiment of the present invention 3, red mud base charcoal to as (v) and as (iii) absorption power
Learn matched curve comparison diagram, wherein: (a) charcoal absorption as (v)；(b) red mud base charcoal absorption as (v)；C () charcoal is inhaled
Attached as (iii)；(d) red mud base charcoal absorption as (iii)；
Fig. 6 is unmodified charcoal in the embodiment of the present invention 4, red mud base charcoal to as (v) and the suction of as (iii) thermodynamics
Attached matched curve comparison diagram, wherein: (a) charcoal absorption as (v)；(b) red mud base charcoal absorption as (v)；C () charcoal is inhaled
Attached as (iii)；(d) red mud base charcoal absorption as (iii).
Specific embodiment
Below by being described in detail to the present invention with specific embodiment in conjunction with the following drawings.
The present invention can obtain charcoal using agriculture waste biomass such as rice straw, straw, kind shells as raw material.
Hereinafter only illustrate taking rice straw as a example.
Red mud used can be using Bayer process, sintering process and combination method (sintering process and Bayer process series, parallel or mixed
Connection) process for making alumina produce solid waste.
Embodiment 1
The red mud base biological carbon materials for arsenic removal of the present embodiment, are prepared from by following steps:
1) rice straw is cleaned remove impurity, pulverize after air-drying, cross 200 mesh sieves, stand-by.
2) certain mass red mud is taken to be added in distilled water (red mud and distilled water solid-to-liquid ratio 1:250g/ml), ultrasound wave is made
Red mud suspension liquor is obtained with 1h.
3) by step 1) the rice straw powder that obtains is added to step 2) red mud suspension liquor that obtains, rice straw with red
Mud mass ratio is 5:1 (red mud is pressed butt and calculated), and stirring and evenly mixing stirs 3h, then carries out standing separation, filters water.
4) by step 3) product that obtains is placed in anoxybiotic roasting in Muffle furnace, is warming up to 600 with the heating rate of 5 DEG C/min
DEG C, and keep 6h at this temperature, it is cooled to room temperature, take out carbonizing production.
5) by step 4) product that obtains cleaned to leacheate 1mol/l agno repeatedly using deionized water3Solution is examined
Survey no cl-And be neutral (ph 7.0 about), dry, you can (red mud-biochar is rm- to prepared red mud base charcoal
bc).
By unmodified charcoal as a comparison, the preparation method of described unmodified charcoal be above-mentioned 1), 4) step, simply
It is added without red mud modified.
Characterization of The Products:
By n2- bet method measures the red mud base charcoal specific surface area difference that unmodified charcoal and the present embodiment are obtained
210.29m2/ g and 186.95m2/ g, the modified charcoal of red mud reduces than the specific surface area of unmodified charcoal, analyzes it
It is likely due to charcoal and has loaded red mud, the presence of red mud covers the hole of charcoal, thus reducing specific surface area.
As is adsorbed by the unmodified charcoal of sem-eds binding analysis and red mud base charcoal and red mud base charcoal
The morphology change of (v) and as (iii) and each element distribution.
From the sem figure of Fig. 1, red mud base charcoal becomes more coarse than unmodified charcoal, surface folding more and
There is granular object, analyze it and be likely due to load red mud.Red mud base charcoal absorption as (v) and as (iii) be not afterwards than
Before absorption, red mud base charcoal surface folding is more.
From the eds figure of Fig. 2, compared with unmodified charcoal, it is new that calcium, aluminum, titanium, sodium, ferrum in red mud base charcoal
Element peak so that it is determined that biological carbon surface has successfully loaded red mud.Before absorption, as element in red mud base charcoal,
The surface of red mud base charcoal has been occurred in thus demonstrating the generation of absorption after absorption.
Unmodified charcoal and the thing phase composition of red mud base charcoal are analyzed by xrd.Fig. 3 show unmodified charcoal
Thing phase composition with red mud base charcoal.
From the figure 3, it may be seen that the mineral composition obvious difference of unmodified charcoal and red mud base charcoal.Red mud base charcoal with
Charcoal is compared, and there is some crystal form mineral such as bloodstone (fe2o3), magnetic iron ore (fe3o4), calcite (caco3), goethitum
(feo (oh)), gibbsite (al (oh)3), perovskite (catio3).Thus further indicate red mud successfully bearing
It is loaded in the surface of charcoal.
Embodiment 1 '
The red mud base biological carbon materials for arsenic removal of the present embodiment, are prepared from by following steps:
1) rice straw is cleaned remove impurity, pulverize after air-drying, cross 80 mesh sieves, stand-by.
2) certain mass red mud is taken to be added in distilled water (red mud and distilled water solid-to-liquid ratio 1:200g/ml), ultrasound wave is made
Red mud suspension liquor is obtained with 30min.
3) by step 1) the rice straw powder that obtains is added to step 2) red mud suspension liquor that obtains, rice straw with red
Mud mass ratio is 3:1 (red mud is pressed butt and calculated), and stirring and evenly mixing stirs 2h, then carries out standing separation, filters water.
4) by step 3) product that obtains is placed in anoxybiotic roasting in Muffle furnace, is warming up to 550 with the heating rate of 4 DEG C/min
DEG C, and keep 8h at this temperature, it is cooled to room temperature, take out carbonizing production.
5) by step 4) product that obtains cleaned to leacheate 1mol/l agno repeatedly using deionized water3Solution is examined
Survey no cl-And be neutral (ph 7.0 about), dry, you can (red mud-biochar is rm- to prepared red mud base charcoal
bc).
Characterization of The Products: specific surface area is 189.8m2/ g, sem-eds and xrd confirm that red mud is supported on the surface of charcoal.
Embodiment 1 "
The red mud base biological carbon materials for arsenic removal of the present embodiment, are prepared from by following steps:
1) rice straw is cleaned remove impurity, pulverize after air-drying, cross 200 mesh sieves, stand-by.
2) certain mass red mud is taken to be added in distilled water (red mud and distilled water solid-to-liquid ratio 1:300g/ml), ultrasound wave is made
Red mud suspension liquor is obtained with 1.5h.
3) by step 1) the rice straw powder that obtains is added to step 2) red mud suspension liquor that obtains, rice straw with red
Mud mass ratio is 7:1 (red mud is pressed butt and calculated), and stirring and evenly mixing stirs 4h, then carries out standing separation, filters water.
4) by step 3) product that obtains is placed in anoxybiotic roasting in Muffle furnace, is warming up to 650 with the heating rate of 6 DEG C/min
DEG C, and keep 5h at this temperature, it is cooled to room temperature, take out carbonizing production.
5) by step 4) product that obtains cleaned to leacheate 1mol/l agno repeatedly using deionized water3Solution is examined
Survey no cl-And be neutral (ph 7.0 about), dry, you can (red mud-biochar is rm- to prepared red mud base charcoal
bc).
Characterization of The Products: specific surface area is 180.05m2/ g, sem-eds and xrd confirm that red mud is supported on the surface of charcoal.
Embodiment 2
The present embodiment is ph to unmodified charcoal, the shadow to as (v) and as (iii) absorption property for the red mud base charcoal
Ring.Unmodified charcoal and red mud base charcoal using embodiment 1 preparation.
Weigh the unmodified charcoal of 0.12g and red mud base charcoal is placed in 50ml centrifuge tube, then be separately added into
30ml10mg/l as (v) and as (iii) solution, use 0.1mol l-1Hcl or naoh adjusts solution ph, is adjusted to different ph values
(2,4,6,8,10,12), are placed on Tempeerature-constant air agitator, are carried out with rotating speed for 200rpm/min in room temperature (25 ± 1 DEG C)
Vibration 24h.After the completion of vibration, filter, in filtrate, arsenic concentration adopts atom fluorimetry.
From Fig. 4 .a, as ph=2, red mud base charcoal absorption as (v) reaches maximal absorptive capacity, and adsorbance is
1622.51μg·g-1.As ph=6, unmodified charcoal absorption as (v) reaches maximum, and it is 481.61 μ g g-1.By scheming
4.b understands it is therefore apparent that unmodified charcoal, red mud base charcoal show similar curve with the change of ph.Totally come
Say, test result indicate that as (v) be easier in the range of acid ph adsorbed, as (iii) in contrast, in alkaline condition
Under be more easily adsorbed.Additionally, red mud base charcoal can significantly improve the absorption to as (v) and as (iii) for the charcoal
Ability.
Embodiment 3
The present embodiment is unmodified charcoal, red mud base charcoal is bent to as (v) and as (iii) dynamic absorption matching
Line.Unmodified charcoal and red mud base charcoal using embodiment 1 preparation.
Weigh the unmodified charcoal of 0.12g and red mud base charcoal is placed in 50ml centrifuge tube, then be separately added into 30ml
10mg/l as (v) and as (iii) solution, use 0.1mol l-1Hcl or naoh adjusts optimal adsorption ph.It is placed in Tempeerature-constant air to shake
Swing device, in room temperature (25 ± 1 DEG C), different time (0.5,1,2,4,8,12,16 and 24h) is carried out for 200rpm/min with rotating speed
Vibration.After the completion of vibration, filter, in filtrate, arsenic concentration adopts atom fluorimetry.
As shown in Figure 5, unmodified charcoal, red mud base charcoal absorption as (v) and as (iii) reach within 24h flat
Weighing apparatus state.Data is fitted find using pseudo-first-order and pseudo-second order kinetic and elovich model, as shown in table 1, does not change
Property charcoal, red mud base charcoal pseudo-second order kinetic model more met to as (v) absorption, correlation coefficient r respectively2For 0.987,
0.957；For the absorption of as (iii), unmodified charcoal absorption as (iii) meets pseudo-second order kinetic model (r2=
0.960), red mud base charcoal absorption as (iii) more meets elovich model (r2=0.962).The red mud base life of load red mud
Thing charcoal, compared with unmodified charcoal, improves to the removal effect of as (iii) and as (v), illustrates red mud base charcoal to water body
Adsorption effect that middle arsenic has had and adsorb stable.
Table 1
Embodiment 4
The present embodiment is unmodified charcoal, red mud base charcoal is bent to as (v) and as (iii) Thermodynamic Adsorption matching
Line.Unmodified charcoal and red mud base charcoal using embodiment 1 preparation.
Weigh the unmodified charcoal of 0.12g and red mud base charcoal is placed in 50ml centrifuge tube, then be separately added at the beginning of 30ml
Beginning concentration is 1-50mg/l as (v) and as (iii) solution, uses 0.1mol l-1Hcl or naoh adjusts optimal adsorption ph.It is placed in
Tempeerature-constant air agitator, carries out vibrating 24h with rotating speed for 200rpm/min in room temperature (25 ± 1 DEG C).After the completion of vibration, mistake
Filter, in filtrate, arsenic concentration adopts atom fluorimetry.
It will be appreciated from fig. 6 that unmodified charcoal, red mud base charcoal increase with the initial concentration of as solution, the absorption of as
Amount dramatically increases first, then progressivelyes reach adsorption equilibrium.Using langmuir and frundlich model, data is fitted
Find, as shown in table 2, charcoal, red mud base charcoal all meet langmuir model to as (v) and as (iii) absorption.Explanation
Red mud base charcoal is adsorbed as monolayer adsorption to as's (iii) and as (v), maximum adsorption capacity respectively 520.0ug/g,
5923.8ug/g.
Table 2
Claims (10)
1. a kind of preparation method of the modification biological Carbon Materials for arsenic removal is it is characterised in that include:
Biomass material powder is added in red mud through ultrasonic disperse and the suspension of water, stirring and evenly mixing and then solid-liquid divides
From；
The roasting under nonoxidizing atmosphere by the biomass obtaining and red mud mixture, 550～650 DEG C of sintering temperature, obtain carbonization
Product, as modification biological Carbon Materials.
2. the modification biological Carbon Materials for arsenic removal according to claim 1 preparation method it is characterised in that: described life
Raw material of substance is rice straw.
3. the modification biological Carbon Materials for arsenic removal according to claim 1 and 2 preparation method it is characterised in that: red
Red mud and distilled water solid-to-liquid ratio 1:200～300g/ml in the suspension of mud and water, biomass material powder with red mud mass ratio is
3～7:1.
4. the modification biological Carbon Materials for arsenic removal according to claim 1 preparation method it is characterised in that: ultrasound wave
Effect 30min～2h is obtained the suspension of red mud and water.
5. the modification biological Carbon Materials for arsenic removal according to claim 1 preparation method it is characterised in that: described stir
Mixing mixing is, stirs 2～4h, then standing separation；The carbonized product deionized water drip washing obtaining removes impurity, using 1mol/l
agno3Solution whether there is cl to detect in leacheate-, and leacheate is neutrality.
6. the modification biological Carbon Materials for arsenic removal according to claim 1 preparation method it is characterised in that: during roasting
It is warming up to 550～650 DEG C with the heating rate of 4～6 DEG C/min, be then incubated 5～8h.
7. the modification biological Carbon Materials for arsenic removal that a kind of preparation method using one of claim 1～6 obtains.
8. a kind of modification biological Carbon Materials for arsenic removal it is characterised in that: bet method measure specific surface area be 180～190m2/
G, has red mud granule in the area load of charcoal, and mineral composition contains fe2o3、fe3o4、caco3、feo(oh)、al(oh)3With
catio3.
9. the modification biological Carbon Materials for arsenic removal according to claim 8 it is characterised in that: its xrd collection of illustrative plates such as accompanying drawing 3
Rm-bc shown in.
10. described in a kind of claim 7 be used for arsenic removal modification biological Carbon Materials application it is characterised in that: for arsenic-containing water
Body arsenic removal, adjusts water body ph 2～6 during absorption as (v), adsorb and adjust water body ph during as (iii) 8～12.
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