CN109796013A - A kind of multistage mesoporous activated carbon and preparation method thereof of the compound bombax cotton preparation of paper mill sludge - Google Patents
A kind of multistage mesoporous activated carbon and preparation method thereof of the compound bombax cotton preparation of paper mill sludge Download PDFInfo
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- CN109796013A CN109796013A CN201811597677.2A CN201811597677A CN109796013A CN 109796013 A CN109796013 A CN 109796013A CN 201811597677 A CN201811597677 A CN 201811597677A CN 109796013 A CN109796013 A CN 109796013A
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Abstract
The invention discloses a kind of multistage mesoporous activated carbon and preparation method thereof of paper mill sludge compound bombax cotton preparation, which includes by bombax cotton and paper mill sludge stirring is compound obtains composite sludge；Desiccation is carried out, take out and is crushed is stand-by；It is added in Carbon Dioxide sodium solution, mixing, which is mixed thoroughly into after pureed impregnates, dries；Baking carbonization is carried out under inert gas protection；Room temperature is cooled to take out later；It carries out levigate after taking-up, washes away extra natrium carbonicum calcinatum and surface residue, and filter drying, cross sieve, Powdered Activated Carbon is made.The present invention is raw material using the compound bombax cotton of paper mill sludge, natrium carbonicum calcinatum is activator, charing and activation heat treatment obtain high performance multi-stage porous absorbent charcoal material simultaneously, it is not only to prepare activated carbon from activated sludge to provide a kind of new idea and method, solve the problems, such as that paper mill sludge processing difficulty is big indirectly, and preparation process is simple and practical, saves energy consumption and time, can be used for producing and applying on a large scale.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of multistage mesoporous activated carbon of the compound bombax cotton preparation of paper mill sludge
And preparation method thereof.
Background technique
It is raw material that active carbon, which is using various biomass, coal and heavy crude, at temperatures of some hundreds of degrees celsius through carbonizing,
A kind of porous Carbon Materials obtained from reactivation.There are a large amount of invisible micropores in absorbent charcoal material, there is prosperity
Internal pore structure and biggish specific surface area, surface also there are a variety of oxygen-containing functional groups, favorable regeneration effect is wide
It is general to be applied to environmental protection, chemical, medical and health, the multiple fields such as food processing and agricultural.Its application field it is continuous
Extension puts forward new requirements the quality of active carbon, handles before raw material to not only promote active carbon, preparation method etc.
The development of aspect also promotes the research and development of different cultivars, property active carbon.For a long time, China with coal or
Timber is the principal item that active carbon made of primary raw material is always in absorbent charcoal material.But the tradition as production active carbon
Raw material timber and coal can not meet demand of the industry to activated carbon application.Moreover, in recent years, with environmental problem and the whole world
Energy problem becomes increasingly conspicuous, and finds new low-cost resource to prepare acticarbon increasingly by vast demanders
Concern.
It results from the sludge of city and industrial waste treatment plant that phosphorus content is more, has and prepare the objective of active carbon
Condition can convert it into active carbon by processing under certain conditions.Paper mill sludge is generated in pulping and papermaking processes
Bulk solid waste, be mainly made of organic matter and inorganic matter.Wherein, organic matter is mainly cellulose, but cellulose with
And lignin etc., inorganic matter mostly come from added various filler (such as alumina, CaCO in pulping and papermaking processes3Deng), apply
Expect (such as kaolin) and other inorganic salts.The complicated component of paper mill sludge, moisture content is high, and processing difficulty is big, currently, enterprise
Mostly use landfill, the mode of air storage or burning is handled, but all there is environment dirts to some extent for these methods
The drawbacks such as dye is serious, occupied space is big, resource utilization is low.
Bombax cotton is a kind of fruit fiber, and hollow tubular is presented.Raw material inherently has higher specific surface area.In recent years
It is mainly used in weaving and adsorbing domain come the research largely for bombax cotton, uses it as biomass carbon material and presoma
It is fewer.But because of the lower reason of bombax cotton specific gravity, yield when being prepared into active carbon is lower to be led to not obtain
It is effective to utilize.
Resource utilization is carried out to paper mill sludge, developing the functionalization product with high added value is academic circles at present
Study more project.In addition, due to containing more carbon in paper mill sludge, it can be used as the raw material for preparing active carbon,
It is a kind of new way of paper mill sludge resource utilization at low cost, solves sludge to society, economic bring immense pressure.And
And there is still a need for further improvements with the absorption property that improves him for paper mill sludge active carbon.
Summary of the invention
Goal of the invention: in view of the problems of the existing technology, the present invention provides a kind of compound bombax cotton system of paper mill sludge
The method of standby multistage mesoporous activated carbon, this method is raw material using the compound bombax cotton of paper mill sludge, and natrium carbonicum calcinatum is activator,
Charing has been carried out simultaneously and activation heat treatment has obtained low cost, and high performance multi-stage porous absorbent charcoal material is not only preparation life
Species activity charcoal provides a kind of new idea and method, solves the problems, such as that paper mill sludge processing difficulty is big indirectly, to making
Paper recycling sludge utilizes and creates a new way.
The present invention also provides more prepared by a kind of method of the compound multistage mesoporous activated carbon of bombax cotton preparation of paper mill sludge
Grade mesoporous activated carbon.
Technical solution: to achieve the goals above, a kind of compound bombax cotton preparation of paper mill sludge is more as described herein
The method of grade mesoporous activated carbon, includes the following steps:
(1) the irregular shearing of bombax cotton to dispersity and paper mill sludge stirring compound is obtained into composite sludge；
(2) composite sludge is subjected to desiccation, takes out and stirs and shear；Desiccation is carried out again, until desiccation is complete, is taken out
And it crushes stand-by；
(3) step (2) is obtained the composite sludge that desiccation crushes to be added in Carbon Dioxide sodium solution, mixing is mixed thoroughly into
Drying obtains the composite sludge of flocculence after pureed dipping；
(4) composite sludge of flocculence is subjected to baking charing under inert gas protection；Room temperature is cooled to take later
Out；
(5) it is levigate to take out the product progress through charing process, and washes away extra natrium carbonicum calcinatum and surface with dust technology
Residue, then be washed with deionized water neutral to pH and filter；
(6) it is dry that filtered product will be taken out, sieve is crossed, Powdered Activated Carbon is made, weigh pack, be put into drying box and save.
Wherein, step (1) the paper mill sludge moisture content is no more than 20%, particle size range 2-5mm.
Wherein, the degree of hollowness of step (1) described bombax cotton is 85~95%, and length is 50~500 μm.
Wherein, step (1) paper mill sludge and bombax cotton volume ratio are 2-4:1.Preferably, paper mill sludge and wood
Cotton fiber volume ratio is 2:1.
Wherein, the mass ratio of step (3) composite sludge and natrium carbonicum calcinatum is 4-5:1, Carbon Dioxide sodium solution
Mass fraction is 20%；Preferably, the mass ratio of composite sludge and natrium carbonicum calcinatum is 4:1.
Wherein, drying is dipping 12-14h after step (3) described dipping, dries 10-12h at 110-120 DEG C.Usually dipping
12h dries 12h at 110 DEG C.
Wherein, step (4) the inert gas purge rate is 120-160mL/min；Inert gas is nitrogen or helium
One of；The baking charing is with 10 DEG C/min temperature programming to 500-700 DEG C of baking 3-4h.
Wherein, step (5) dust technology is concentration 1.1-1.3mol/L nitric acid solution.
The compound bombax cotton of paper mill sludge of the present invention prepares multi-stage porous prepared by the method for multistage mesoporous activated carbon
Active carbon.
Wherein, multistage mesoporous activated carbon specific surface area is 2000-2500m2/ g or more, pore-size distribution mainly 0.5-4nm it
Between, for average pore size in 3nm or so, methylene blue adsorption value is 200~250mg/g, and iodine absorption number is 1200~1500mg/g, first
The adsorption capacity of benzene is 160~200mg/g.
The present invention is to supplement bombax cotton and implement the shortcomings that when active carbon is prepared separately in paper mill sludge.Individually
Paper mill sludge can be lost partial organic substances matter during dehydration from water, cause the active carbon specific surface area and absorption of preparation
Rate is lower, and compound bombax cotton can both retain the stream of organic matter in sludge by bombax cotton to the strong adsorption capacity of organic matter
Lose the poor quality for avoiding and preparing active carbon in the process because few charcoal problem causes active carbon.
The utility model has the advantages that compared with prior art, the present invention has the effect that
The invention discloses the methods that a kind of compound bombax cotton of paper mill sludge prepares multistage mesoporous activated carbon, and the present invention is to make
As raw material, addition natrium carbonicum calcinatum is activator for paper sludge and bombax cotton, has carried out charing and activation heat treatment preparation is more
Grade mesoporous activated carbon.Wherein, bombax cotton both can retain organic matter in sludge by strong adsorption capacity of the bombax cotton to organic matter
Loss avoid preparing few charcoal problem during active carbon, while also act addition carbon source effect.
Preparation method simple process of the present invention, it is easy to implement, it can effectively increase the specific surface area of Carbon Materials, and make it
Rich in micropore, and products collection efficiency is high, overcomes when being prepared into active carbon using bombax cotton specific gravity is lower that yield is lower to be caused
The problem of being unable to get effective utilization is a kind of new method for preparing biomass multistage mesoporous activated carbon, for low cost, high-performance
The preparation of biomass multistage mesoporous activated carbon provide new simple approach, be expected to expand its application field.
Multi-stage porous activated carbon raw material large specific surface area prepared by the present invention, pore-size distribution is wide, there is the presence of macropore and aperture,
It is significant for methylene blue adsorption number and iodine adsorption effect, it is excellent for the adsorption rate of toluene.
Detailed description of the invention
Fig. 1 is bombax cotton scanning electron microscopic picture used in the embodiment of the present invention 1；
Fig. 2 is the multistage hole data and graph of pore diameter distribution that active carbon is prepared in the embodiment of the present invention 1；
Fig. 3 is the SEM figure that active carbon is prepared in the embodiment of the present invention 1.
Specific embodiment
The invention will be further described With reference to embodiment.
Embodiment 1
(1) compound, mixing time 15min is stirred into the irregular shearing of bombax cotton to dispersity and paper mill sludge,
Until stirring extent is uniform, composite sludge is obtained；Bombax cotton degree of hollowness is 90%, and length is 250 μm or so；Papermaking is dirty
The moisture content 20% of mud, particle size range are 3mm or so；Sludge and the compound volume ratio of kapok are 2:1；
(2) composite sludge is sent into desiccation in rotary drying machine, takes out and stirs and suitably shear；It is sent into drying again
Machine carries out desiccation, until complete desiccation, takes out and crush stand-by；
(3) it is 4:1 according to the mass ratio of composite sludge and natrium carbonicum calcinatum, is answered what step (3) obtained that desiccation crushes
It closes sludge to be added in Carbon Dioxide sodium solution, pureed dipping 12h is mixed into mixing thoroughly, is dried 12h at 110 DEG C, is obtained flocculence
Composite sludge；
(4) composite sludge of flocculence is sent into carbonizer, under inert gas protection, purge rates 140mL/
min；Inert gas is nitrogen, with 10 DEG C/min temperature programming to 600 DEG C of baking 3h；It is taken after being cooled to room temperature to carbonizer
Out；
(5) it is levigate in crucible to take out the product through charing process, and is washed away with 1.2mol/L dust technology extra anhydrous
Sodium carbonate and surface residue, then be washed with deionized water neutral to pH and filter；
(6) 3h dry in 120 DEG C of filtered product of pumping of drying box is finished, makes it through 0.15mm sieve, powder is made
Active carbon weighs pack, is put into drying box and saves up to multistage mesoporous activated carbon.
Multistage mesoporous activated carbon specific surface area manufactured in the present embodiment is 2500m2/ g or so, pore-size distribution is mainly in 0.5-
Between 4nm, average pore size is in 3nm or so, methylene blue adsorption value 250mg/g, iodine absorption number 1500mg/g, the suction of toluene
Attached capacity is 200mg/g.
The bombax cotton scanning electron microscopic picture used in the present embodiment is as shown in Figure 1；Active carbon is prepared in the present invention
Multistage hole data and graph of pore diameter distribution are as shown in Figure 2；The SEM figure for preparing active carbon is as shown in Figure 3.
Embodiment 2
(1) compound, mixing time 20min is stirred into the irregular shearing of bombax cotton to dispersity and paper mill sludge,
Until stirring extent is uniform, composite sludge is obtained；Bombax cotton degree of hollowness is 95%, and length is 500 μm or so；Papermaking is dirty
The moisture content 15% of mud, particle size range are 2mm or so；Sludge and the compound volume ratio of kapok are 4:1；
(2) composite sludge is sent into desiccation in rotary drying machine, takes out and stirs and suitably shear；It is sent into drying again
Machine carries out desiccation, until complete desiccation, takes out and crush stand-by；
(3) it is 5:1 according to the mass ratio of composite sludge and natrium carbonicum calcinatum, is answered what step (3) obtained that desiccation crushes
It closes sludge to be added in Carbon Dioxide sodium solution, pureed dipping 14h is mixed into mixing thoroughly, is dried 10h at 120 DEG C, is obtained flocculence
Composite sludge；
(4) composite sludge of flocculence is sent into carbonizer, under inert gas protection, purge rates 160mL/
min；Inert gas is nitrogen, with 10 DEG C/min temperature programming to 500 DEG C of baking 4h；It is taken after being cooled to room temperature to carbonizer
Out；
(5) it is levigate in crucible to take out the product through charing process, and is washed away with 1.1mol/L dust technology extra anhydrous
Sodium carbonate and surface residue, then be washed with deionized water neutral to pH and filter；
(6) 3h dry in 120 DEG C of filtered product of pumping of drying box is finished, makes it through 0.15mm sieve, powder is made
Active carbon weighs pack, is put into drying box and saves up to multistage mesoporous activated carbon.
Multistage mesoporous activated carbon specific surface area manufactured in the present embodiment is 2200m2/ g or so, pore-size distribution is mainly in 0.5-
Between 4nm, average pore size is in 3nm or so, methylene blue adsorption value 200mg/g, iodine absorption number 1200mg/g, the suction of toluene
Attached capacity is 180mg/g.
Embodiment 3
(1) compound, mixing time 10min is stirred into the irregular shearing of bombax cotton to dispersity and paper mill sludge,
Until stirring extent is uniform, composite sludge is obtained；Bombax cotton degree of hollowness is 85%, and length is 50 μm or so；Papermaking is dirty
The moisture content 20% of mud, particle size range are 5mm or so；Sludge and the compound volume ratio of kapok are 4:1；
(2) composite sludge is sent into desiccation in rotary drying machine, takes out and stirs and suitably shear；It is sent into drying again
Machine carries out desiccation, until complete desiccation, takes out and crush stand-by；
(3) it is 5:1 according to the mass ratio of composite sludge and natrium carbonicum calcinatum, is answered what step (3) obtained that desiccation crushes
It closes sludge to be added in Carbon Dioxide sodium solution, pureed dipping 14h is mixed into mixing thoroughly, is dried 10h at 120 DEG C, is obtained flocculence
Composite sludge；
(4) composite sludge of flocculence is sent into carbonizer, under inert gas protection, purge rates 120mL/
min；Inert gas is nitrogen, with 10 DEG C/min temperature programming to 700 DEG C of baking 3h；It is taken after being cooled to room temperature to carbonizer
Out；
(5) it is levigate in crucible to take out the product through charing process, and is washed away with 1.3mol/L dust technology extra anhydrous
Sodium carbonate and surface residue, then be washed with deionized water neutral to pH and filter；
(6) 3h dry in 120 DEG C of filtered product of pumping of drying box is finished, makes it through 0.15mm sieve, powder is made
Active carbon weighs pack, is put into drying box and saves up to multistage mesoporous activated carbon.
Multistage mesoporous activated carbon specific surface area manufactured in the present embodiment is 2000m2/ g or so, pore-size distribution is mainly in 0.5-
Between 4nm, for average pore size in 3nm or so, methyl blue adsorptive value is 220mg/g, iodine absorption number 1300mg/g, the absorption of toluene
Capacity is 160mg/g.
Test example 1
The active carbon items of the multistage mesoporous activated carbon prepared and each comparative example in the test present invention under the same conditions
Energy index, test active carbon specific surface area, methylene blue adsorption value, iodine absorption number, toluene adsorbance etc. the results are shown in Table 1.
Methylene blue adsorption value detection: weighing dry sample 0.1g, (scale standard to 1mg) is placed in the cone of 100mL tool grinding port plug
In shape flask, suitable methylene blue test liquid is added with buret, after sample is all wet, is immediately placed on concussion 20min,
Environment temperature (25 ± 5) DEG C, is filtered with filter paper.Filtrate is placed in the cuvette that optical path is 25px, uses spectrophotometric
Meter measures absorbance at wavelength 665m, (weighs 4.000g cupric sulfate crystals (Cu2SO4 with copper sulphate standard colour filter liquid
5H2O) be dissolved in 1000mL water) absorbance contrast, consumed methylene blue test liquid measure is the methylene blue of sample
Adsorptive value, methylene blue adsorption value are indicated as unit of mg/g.
Iodine absorption number detection: GB/T 12496.8-2015 wood activated charcoal test method, the measurement of iodine sorption value are referred to.
The detection of toluene adsorbance: GB/T 35815-2018 wood activated charcoal test method, the survey of toluene adsorption rate are referred to
It is fixed.
Wherein: comparative example 1 is using 1 preparation method of embodiment, the difference is that being added without kapok fibre in step (1)
Dimension.
Comparative example 2 is using 1 preparation method of embodiment, the difference is that being added without paper mill sludge in step (1).
Comparative example 3 uses the preparation side of the biomass porous carbon plate based on bombax cotton disclosed in patent CN107098327A
The biomass porous carbon plate that method and application obtain.
Comparative example 4 is living using a kind of sludge that the preparation method of active sludge carbon obtains disclosed in patent CN106927462A
Property charcoal.
The multistage mesoporous activated carbon performance indexes of table 1
The multistage mesoporous activated carbon of preparation of the embodiment of the present invention does not add bombax cotton or papermaking compared with comparative example 1 and 2
The indices of sludge obviously not as good as the multistage mesoporous activated carbon of paper mill sludge of the present invention compound bombax cotton preparation, while with show
There is technology to compare, the preparation process of biomass porous carbon plate of the comparative example 3 based on bombax cotton is totally different from the present invention, preparation
The most of specific surface areas of porous carbon plate in 1000m2/ g, other indexs are also not so good as multistage mesoporous activated carbon prepared by the present invention,
Active sludge carbon indices prepared by comparative example 4 are also not so good as performance indexes of the invention.
Claims (10)
1. a kind of method that the compound bombax cotton of paper mill sludge prepares multistage mesoporous activated carbon, which comprises the steps of:
(1) the irregular shearing of bombax cotton to dispersity and paper mill sludge stirring compound is obtained into composite sludge；
(2) composite sludge is subjected to desiccation, takes out and stirs and shear；Desiccation is carried out again, until desiccation is complete, takes out simultaneously powder
It is broken stand-by；
(3) step (2) is obtained the composite sludge that desiccation crushes to be added in Carbon Dioxide sodium solution, pureed is mixed into mixing thoroughly
Drying obtains the composite sludge of flocculence after dipping；
(4) composite sludge of flocculence is subjected to baking charing under inert gas protection；Room temperature is cooled to take out later；
(5) it is levigate to take out the product progress through charing process, and washes away extra natrium carbonicum calcinatum and remained on surface with dust technology
Object, then be washed with deionized water neutral to pH and filter；
(6) it is dry that filtered product will be taken out, sieve is crossed, Powdered Activated Carbon is made, weigh pack, be put into drying box and save.
2. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In step (1) the paper mill sludge moisture content is no more than 20%, particle size range 2-5mm.
3. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In the degree of hollowness of step (1) described bombax cotton is 85~95%, and length is 50~500 μm.
4. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In step (1) paper mill sludge and bombax cotton volume ratio are 2~4:1.
5. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In the mass ratio of step (3) composite sludge and Carbon Dioxide sodium solution is 4~5:1.
6. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In drying is 12~14h of dipping after step (3) described dipping, dries 10~12h at 110-120 DEG C.
7. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In step (4) the inert gas purge rate is 120-160mL/min；Inert gas is one of nitrogen or helium；Institute
Baking carbonization is stated with 10 DEG C/min temperature programming to 500-700 DEG C of 3~4h of baking.
8. the method that the compound bombax cotton of paper mill sludge according to claim 1 prepares multistage mesoporous activated carbon, feature exist
In step (5) described dust technology is preferably concentration 1.1~1.3mol/L nitric acid solution.
9. a kind of compound bombax cotton of paper mill sludge described in claim 1 prepares more prepared by the method for multistage mesoporous activated carbon
Grade mesoporous activated carbon.
10. it is according to claim 9 multistage mesoporous activated carbon, which is characterized in that it is described multistage mesoporous activated carbon specific surface area be
2000-2500m2/ g or more, pore-size distribution is mainly between 0.5-4nm, and average pore size is in 3nm or so, methylene blue adsorption value
For 200~250mg/g, iodine absorption number is 1200~1500mg/g, and the adsorption capacity of toluene is 160~200mg/g.
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Cited By (1)
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| CN114772576A (en) * | 2022-04-28 | 2022-07-22 | 南京信息工程大学 | Method for preparing carbon material from wood block |
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