CN108862277A - Rice husk-sludge base composite activated carbon and preparation method thereof - Google Patents
Rice husk-sludge base composite activated carbon and preparation method thereof Download PDFInfo
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- CN108862277A CN108862277A CN201810961042.XA CN201810961042A CN108862277A CN 108862277 A CN108862277 A CN 108862277A CN 201810961042 A CN201810961042 A CN 201810961042A CN 108862277 A CN108862277 A CN 108862277A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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Abstract
The invention discloses a kind of rice husk-sludge base composite activated carbons and preparation method thereof, which includes：(1) sludge is dried, is crushed, the sludge that obtains that treated；(2) treated sludge is uniformly mixed with dry rice husk, after then mixing, impregnating with activator, is dried, obtains mixture；(3) in the presence of protective gas, mixture is subjected to carbonization treatment；(4) mixture after step (3) carbonization treatment is washed to pH value is neutrality, dry, broken, and rice husk-sludge base composite activated carbon is made.Compared with traditional sludge matrix activated carbon, yield increases rice husk of the invention-sludge base composite activated carbon, and specific surface area increases, and micropore ratio increases, and average pore size increases；Obtained rice husk-sludge base composite activated carbon yield can reach 88.09%, specific surface area 435.58m2/ g, micropore ratio are 41.25%, average pore size 5.33nm.
Description
Technical field
The invention belongs to technical field of sludge treatment, more particularly, to a kind of rice husk-sludge base composite activated carbon and its
Preparation method.
Background technique
Sludge is the product after sewage treatment, the pole being made of organic debris, microorganism, inorganic particle, colloid etc.
Its complicated heterogeneous body, moisture content is high, high organic content, it is smelly to be easy corruption, and particle is thinner, and specific gravity is smaller,
Jelly liquid.It is the concentrated thing between liquid and solid, is difficult to be separated by solid-liquid separation by sedimentation.In China's sewage
In treatment process, " the light mud of heavy water " phenomenon generally existing for a long time, so that wastewater treatment in China is fast-developing, but at sludge
Reason industry is but stagnated.Contain a large amount of organic matter in sludge, there is the objective condition for being processed to carbon-bearing adsorbent, utilizes
Sludge prepares active carbon, can not only utilize recycling sludge, and can also obtain inexpensive active carbon, by sludge-based activated carbon
For making adsorbent with huge application prospect.
Currently, being chemical activation method by the common method that sludge is prepared as active carbon, sludge and chemical activating agent are pressed one
After fixed ratio is mixed and impregnated, is carbonized under the conditions of anoxybiotic environment and certain temperature, finally obtain activated carbon product.
The yield of the active carbon of this method is higher, and activator can recycle, and charing synchronous can be carried out with activation process, and living
Change temperature is lower, can be realized in process of production by the concentration of the type of control activator, dosage and activator certain
Degree on control the pore-size distribution of finished activated charcoal.But active carbon is prepared currently with sludge there are the following problems：(1) by
It is lower in the phosphorus content of raw material sludge, content of ashes is higher, with conventional wooden active carbon, active carbon from coal compare, sludge base
The yield of active carbon is not high, and application is not strong；(2) exist using sludge-based activated carbon made from the prior art (chemical activation method)
The problem that specific surface area is small, micropore ratio is low.
Summary of the invention
The purpose of the present invention is overcoming the deficiencies of existing technologies, a kind of preparation of rice husk-sludge base composite activated carbon is provided
Method makes rice husk-sludge base of preparation by adulterating rice husk into sludge to improve the phosphorus content of sludge raw material, reduce ash content
Composite activated carbon yield, specific surface area and micropore ratio increase.
To achieve the goals above, an aspect of of the present present invention provides a kind of preparation side of rice husk-sludge base composite activated carbon
Method, which is characterized in that the preparation method includes the following steps：
(1) sludge is dried, is crushed, the sludge that obtains that treated；
(2) treated the sludge is uniformly mixed with dry rice husk, after then mixing, impregnating with activator, into
Row drying, obtains mixture；
(3) in the presence of protective gas, the mixture is subjected to carbonization treatment；
(4) mixture after step (3) described carbonization treatment is washed to pH value is neutrality, dry, broken, is made described
Rice husk-sludge base composite activated carbon.
Another aspect of the present invention provides a kind of rice husk-sludge base composite activated carbon of above-mentioned preparation method preparation.
Rice husk of the invention-sludge base composite activated carbon is compared with traditional sludge matrix activated carbon, and yield increases, specific surface area
Increase, micropore ratio increases, and average pore size increases；Obtained rice husk-sludge base composite activated carbon yield can reach
88.09%, specific surface area 435.58m2/ g, micropore ratio are 41.25%, average pore size 5.33nm.
Other features and advantages of the present invention will then part of the detailed description can be specified.
Detailed description of the invention
Exemplary embodiment of the invention is described in more detail in conjunction with the accompanying drawings, it is of the invention above-mentioned and its
Its purpose, feature and advantage will be apparent, wherein in exemplary embodiment of the invention, identical reference label
Typically represent same parts.
Fig. 1 shows rice husk-sludge base composite activated carbon scanning electron microscope (SEM) photograph of embodiment according to the present invention 5.
Fig. 2 shows the scanning electron microscope (SEM) photographs of the sludge-based activated carbon of comparative example 1 according to the present invention.
Specific embodiment
The preferred embodiment of the present invention is described in more detail below.Although the following describe preferred implementations of the invention
Mode, however, it is to be appreciated that may be realized in various forms the present invention without that should be limited by the embodiments set forth herein.Phase
Instead, these embodiments are provided so that the present invention is more thorough and complete, and can be by the scope of the present invention completely
It is communicated to those skilled in the art.
An aspect of of the present present invention provides a kind of preparation method of rice husk-sludge base composite activated carbon, which includes
Following steps：
(1) sludge is dried, is crushed, the sludge that obtains that treated；
(2) treated the sludge is uniformly mixed with dry rice husk, after then mixing, impregnating with activator, into
Row drying, obtains mixture；
(3) in the presence of protective gas, the mixture is subjected to carbonization treatment；
(4) mixture after step (3) described carbonization treatment is washed to pH value is neutrality, dry, broken, is made described
Rice husk-sludge base composite activated carbon.
In accordance with the present invention it is preferred that the activator be mass concentration be 40-60% phosphate aqueous solution, potassium hydroxide
At least one of aqueous solution and solder(ing)acid.
In accordance with the present invention it is preferred that the temperature of the drying is 100-110 DEG C in step (1)；It is described that treated is dirty
The average grain diameter of mud is not more than 1mm.
In accordance with the present invention it is preferred that in step (2), the mass ratio of treated the sludge and dry rice husk is 1:
1-3；The mass ratio of the mixture and the activator of treated the sludge and dry rice husk is 1:1-3.
In accordance with the present invention it is preferred that the time of the dipping is 20-28h, and the temperature of the drying is in step (2)
100-110℃。
In accordance with the present invention it is preferred that the protective gas is nitrogen, and the carbonization treatment is in tube type vacuum in step (3)
It is carried out in furnace, the temperature of the carbonization treatment is 400-600 DEG C, time 1.5-3h, and heating rate is 3-7 DEG C/min.
In accordance with the present invention it is preferred that the temperature of the drying is 100-110 DEG C, the rice husk-sludge base in step (4)
Composite activated carbon average grain diameter is not more than 1mm.
In the present invention, being crushed device used is preferably ball mill.
Another aspect of the present invention provides a kind of rice husk-sludge base composite activated carbon of above-mentioned preparation method preparation.
The present invention is further illustrated by the following examples：
Embodiment 1
The present embodiment provides a kind of rice husk-sludge base composite activated carbon preparation methods, and specific step is as follows：
(1) sludge is put into air dry oven, is arranged 105 DEG C of temperature, drying to constant weight is drawn off, will with ball mill
Dry sludge carries out break process until small graininess, crosses after 1mm sieve the sludge that is made that treated, is stored in plastic packaging bag
Middle sealed storage；
(2) rice husk is put into air dry oven, is arranged 105 DEG C of temperature, drying is drawn off to constant weight, obtains drying
Rice husk is stored in sealed storage in plastic packaging bag；
It (3) is in mass ratio 1 by the rice husk of treated sludge, drying:1 is uniformly mixed, and takes aggregate sample and mass concentration
Phosphate aqueous solution for 50% is 1 in mass ratio:1 mixing, the drying box under the conditions of dipping is put into 105 DEG C for 24 hours afterwards are dried,
To constant weight, mixture is obtained；Appropriate mixture is weighed, quartz boat is put into, quartz boat is put into tube type vacuum furnace.
(4) N is passed through into tube type vacuum furnace2, drain air, in N2Protect atmosphere under, control heating rate be 5 DEG C/
Min is warming up to 400 DEG C of set temperature, and constant temperature 2h is kept to carry out carbonization treatment.
(5) distilled water is added into the mixture after carbonization treatment, will be washed to pH value repeatedly for neutrality, after finally washing
Substance be put in 105 DEG C of baking ovens and dry to constant weight, taking-up is put in drier cooling, was crushed 1mm sieve, and obtained rice husk-dirt
Mud base composite activated carbon.
Embodiment 2
The present embodiment and embodiment 1 are distinguished as in step (3), by treated sludge, drying rice husk in mass ratio
It is 1:3 are uniformly mixed；Other each processing steps, technological parameter and substance used and dosage are same as Example 1.
Embodiment 3
The present embodiment provides a kind of rice husk-sludge base composite activated carbon preparation methods, and specific step is as follows：
(1) sludge is put into air dry oven, is arranged 105 DEG C of temperature, drying to constant weight is drawn off, will with ball mill
Dry sludge carries out break process until small graininess, crosses after 1mm sieve the sludge that is made that treated, is stored in plastic packaging bag
Middle sealed storage；
(2) rice husk is put into air dry oven, is arranged 105 DEG C of temperature, drying is drawn off to constant weight, obtains drying
Rice husk is stored in sealed storage in plastic packaging bag；
It (3) is in mass ratio 1 by the rice husk of treated sludge, drying:1 is uniformly mixed, and takes aggregate sample and mass concentration
Potassium hydroxide aqueous solution for 50% is 1 in mass ratio:1 mixing, the drying box under the conditions of dipping is put into 105 DEG C for 24 hours afterwards carry out
It is dry, until constant weight, obtains mixture；Appropriate mixture is weighed, quartz boat is put into, quartz boat is put into tube type vacuum furnace.
(4) N is passed through into tube type vacuum furnace2, drain air, in N2Protect atmosphere under, control heating rate be 5 DEG C/
Min is warming up to 400 DEG C of set temperature, and constant temperature 2h is kept to carry out carbonization treatment.
(5) distilled water is added into the mixture after carbonization treatment, will be washed to pH value repeatedly for neutrality, after finally washing
Substance be put in 105 DEG C of baking ovens and dry to constant weight, taking-up is put in drier cooling, was crushed 1mm sieve, and obtained rice husk-dirt
Mud base composite activated carbon.
Embodiment 4
The present embodiment and embodiment 3 are distinguished as in step (3), by treated sludge, drying rice husk in mass ratio
It is 1:1 is uniformly mixed, and the potassium hydroxide aqueous solution for taking aggregate sample to be 50% with mass concentration is 1 in mass ratio:3 mixing；It is other
Each processing step, technological parameter and substance used and dosage are same as Example 3.
Embodiment 5
The present embodiment provides a kind of rice husk-sludge base composite activated carbon preparation methods, and specific step is as follows：
(1) sludge is put into air dry oven, is arranged 105 DEG C of temperature, drying to constant weight is drawn off, will with ball mill
Dry sludge carries out break process until small graininess, crosses after 1mm sieve the sludge that is made that treated, is stored in plastic packaging bag
Middle sealed storage；
(2) rice husk is put into air dry oven, is arranged 105 DEG C of temperature, drying is drawn off to constant weight, obtains drying
Rice husk is stored in sealed storage in plastic packaging bag；
It (3) is in mass ratio 1 by the rice husk of treated sludge, drying:1 is uniformly mixed, and takes aggregate sample and mass concentration
Solder(ing)acid for 50% is 1 in mass ratio:1 mixing, the drying box under the conditions of dipping is put into 105 DEG C for 24 hours afterwards are done
It is dry, until constant weight, obtains mixture；Appropriate mixture is weighed, quartz boat is put into, quartz boat is put into tube type vacuum furnace.
(4) N is passed through into tube type vacuum furnace2, drain air, in N2Protect atmosphere under, control heating rate be 5 DEG C/
Min is warming up to 400 DEG C of set temperature, and constant temperature 2h is kept to carry out carbonization treatment.
(5) distilled water is added into the mixture after carbonization treatment, will be washed to pH value repeatedly for neutrality, after finally washing
Substance be put in 105 DEG C of baking ovens and dry to constant weight, taking-up is put in drier cooling, was crushed 1mm sieve, and obtained rice husk-dirt
Mud base composite activated carbon.
Embodiment 6
The present embodiment is distinguished as in step (4) with embodiment 5, is warming up to 600 DEG C of set temperature；Other each technique steps
Suddenly, technological parameter and substance used and dosage are same as Example 5.
Comparative example 1
This comparative example provides a kind of preparation method of sludge-based activated carbon, and specific step is as follows：
(1) sludge is put into air dry oven, is arranged 105 DEG C of temperature, drying to constant weight is drawn off, will with ball mill
Dry sludge carries out break process until small graininess, crosses after 1mm sieve the sludge that is made that treated, is stored in plastic packaging bag
Middle sealed storage；
It (2) is in mass ratio 1 by treated sludge and the solder(ing)acid that mass concentration is 50%:1 mixing, dipping
Drying box under the conditions of being put into 105 DEG C afterwards for 24 hours is dried, until constant weight, obtains mixture；Appropriate mixture is weighed, stone is put into
Quartz boat is put into tube type vacuum furnace by Ying Zhou.
(4) N is passed through into tube type vacuum furnace2, drain air, in N2Protect atmosphere under, control heating rate be 5 DEG C/
Min is warming up to 400 DEG C of set temperature, and constant temperature 2h is kept to carry out carbonization treatment.
(5) distilled water is added into the mixture after carbonization treatment, will be washed to pH value repeatedly for neutrality, after finally washing
Substance be put in 105 DEG C of baking ovens and dry to constant weight, taking-up is put in drier cooling, was crushed 1mm sieve, it is living to obtain sludge base
Property charcoal.
Comparative example 2
This comparative example and embodiment 3 are distinguished as in step (3), by treated sludge, drying rice husk in mass ratio
It is 1:4 are uniformly mixed；Other each processing steps, technological parameter and substance used and dosage are same as Example 3.
Comparative example 3
This comparative example and embodiment 3 are distinguished as in step (3), by treated sludge, drying rice husk in mass ratio
It is 1:1 is uniformly mixed, and the potassium hydroxide aqueous solution for taking aggregate sample to be 50% with mass concentration is 1 in mass ratio:4 mixing；It is other
Each processing step, technological parameter and substance used and dosage are same as Example 3.
Comparative example 4
This comparative example is distinguished as in step (4) with embodiment 3, is warming up to 350 DEG C of set temperature；Other each technique steps
Suddenly, technological parameter and substance used and dosage are same as Example 3.
Comparative example 5
This comparative example is distinguished as in step (4) with embodiment 3, is warming up to 650 DEG C of set temperature；Other each technique steps
Suddenly, technological parameter and substance used and dosage are same as Example 3.
Test case 1
Yield, specific surface area, micropore ratio and the average hole of the active carbon of testing example 1-6 and comparative example 1-5 preparation
Diameter, concrete outcome are shown in Table 1.
Wherein, according to《Gas absorption BET method measures solid matter specific surface area》(GB/T19587-2017), using JW-
BK atmosphere of static nitrogen adsorption instrument (the precise and tiny Gao Bo Science and Technology Ltd. in Beijing) detects the specific surface area of active carbon, micropore ratio and average
Aperture.Wherein, the nitrogen that the adsorbing medium of test is 99.99%, sample are in liquid nitrogen saturation temperature condition, relative pressure P/P0
Between 0.01 to 0.995, measurement accuracy<± 2%, pressure controling precision 0.2%.
Table 1
Test case 2
To embodiment 5 prepare rice husk-sludge base composite activated carbon and comparative example 1 prepare sludge-based activated carbon respectively into
Row electron-microscope scanning obtains rice husk-sludge base composite activated carbon and sludge-based activated carbon microstructure scanning electron microscope (SEM) photograph.
As shown in Figs. 1-2, by the analysis of scanning electron microscopic picture as can be seen that structure as shown in Figure 1 is mainly with honeycomb
Based on shape structure, specimen surface is coarse, and inside forms the porous structure of carbon skeleton, and particulate units body is based on sheet.Such as
Shown in Fig. 2, for sample based on laminated structure, there are irregular ghost mineral on surface, and overlap joint at random stacks between each other, is in nothing
Sequence arrangement, without obvious cellular structure.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes are obvious for the those of ordinary skill in art field.
Claims (8)
1. a kind of rice husk-sludge base composite activated carbon preparation method, which is characterized in that the preparation method includes the following steps：
(1) sludge is dried, is crushed, the sludge that obtains that treated；
(2) treated the sludge is uniformly mixed with dry rice husk, after then mixing, impregnating with activator, is done
It is dry, obtain mixture；
(3) in the presence of protective gas, the mixture is subjected to carbonization treatment；
(4) mixture after step (3) described carbonization treatment is washed to pH value is neutrality, dry, broken, and the rice is made
Shell-sludge base composite activated carbon.
2. the preparation method according to weighing and require 1, wherein the activator is that the phosphoric acid that mass concentration is 40-60% is water-soluble
At least one of liquid, potassium hydroxide aqueous solution and solder(ing)acid.
3. the preparation method according to weighing and require 1, wherein in step (1), the temperature of the drying is 100-110 DEG C；It is described
The average grain diameter of treated sludge is not more than 1mm.
4. according to power require 1 described in preparation method, wherein in step (2), treated the sludge and dry rice husk
Mass ratio is 1:1-3；The mass ratio of the mixture and the activator of treated the sludge and dry rice husk is 1:1-
3。
5. the preparation method according to weighing and require 1, wherein in step (2), the time of the dipping is 20-28h, described dry
Dry temperature is 100-110 DEG C.
6. according to power require 1 described in preparation method, wherein in step (3), the protective gas is nitrogen, at the carbonization
Reason carries out in tube type vacuum furnace, and the temperature of the carbonization treatment is 400-600 DEG C, time 1.5-3h, heating rate 3-7
℃/min。
7. the preparation method according to weighing and require 1, wherein in step (4), the temperature of the drying is 100-110 DEG C, described
Rice husk-sludge base composite activated carbon average grain diameter is not more than 1mm.
8. rice husk-sludge base composite activated carbon that power requires preparation method described in any one of 1-7 to prepare.
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| CN113753895A (en) * | 2021-08-25 | 2021-12-07 | 海南大学 | Method for preparing activated carbon by using areca and sludge as materials |
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Application publication date: 20181123 |