CN107986275A - A kind of production method of biological activated carbon - Google Patents
A kind of production method of biological activated carbon Download PDFInfo
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- CN107986275A CN107986275A CN201711414517.5A CN201711414517A CN107986275A CN 107986275 A CN107986275 A CN 107986275A CN 201711414517 A CN201711414517 A CN 201711414517A CN 107986275 A CN107986275 A CN 107986275A
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Abstract
The invention discloses a kind of production method of biological activated carbon, comprise the following steps that:Catalyst is added into boiling solvent, and adds plant fiber material and carries out boiling processing;Separation of solid and liquid is carried out after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;Under conditions of 200 DEG C by plant fiber drying to moisture 20% within;Under conditions of 400 ~ 600 °C, fibrous raw material is carbonized, carbonization time is 10 ~ 30min, obtains carbide;Activator is added, activator is mixed and crushed with carbide, is activated under conditions of 700 ~ 900 DEG C, soak time is 30 ~ 120min;Adopt that to be washed with deionized to pH value be 5 ~ 7, dry 3 10min, are cooled to room temperature, obtain product under the conditions of 200 DEG C.The present invention has the advantages that quality is good, effect is good.
Description
Technical field
The present invention relates to biomass chemical field, more particularly to a kind of production method of biological activated carbon.
Background technology
Activated carbon is a kind of excellent sorbing material, is widely used in the every field such as pharmacy, chemical industry, food, metallurgy.
Conventional method is generally used as raw materials for production using timber, cocoanut shell, fruit stone, bagasse, fat coal etc., due to high-quality
Coal is of high cost, so more economic production method uses plant fiber material more, conventional method mainly has following shortcoming:
Plant fiber material grades impurity wherein comprising lignin, cellulose, three big component of hemicellulose containing ash, wherein wooden
Carbon content is high in quality, cellulose, it is also the important composition for preparing activated carbon, but hemi-cellulose components have to preparing activated carbon
Inhibitory action, especially influences activation effect.Hemi-cellulose components content is above 20% in most plants raw material, if by original
Expect unprocessed(Still contain a large amount of hemicelluloses)In the case of be directly used in production activated carbon, then product activation effect is bad, most
Product quality is influenced eventually;
Except the fabulous wood raw material of quality(The timber such as needlebush, leaf wood)Outside, more ash is generally contained in plant fiber material
Point, but content of ashes can directly affect content of ashes in activated carbon product in raw material, if preparing activity using high-quality timber
Charcoal, cost are high;According to lower-cost plant fiber material(Such as cocoanut shell, fruit stone, bagasse), then often ash content contains
Amount is higher, if unprocessed directly produce activated carbon, content of ashes also can be higher in product;
In plant fiber material, lignin is crosslinked mutually with cellulosic structure, and contact is close, if failing to tie both before activation
Structure suitably disperse, then due to the influence of lignin, the activated carbon product specific surface area of output is often smaller, adsorption effect
It is bad, if but be kept completely separate out by lignin therein, lignin " has been wasted " again, because lignin carbon content is very high, this
Body is also to prepare the good raw material of activated carbon, so cellulose and lignin separation both can guarantee that to a suitable degree
Activated carbon product specific surface area is big, can also ensure high yield pulp1 as far as possible, is always a problem.
, it is necessary to additionally add the complicated activation such as clay, waterborne polyurethane resin, zinc chloride in the production method of other part
Agent or catalyst, while production cost further increases, also to introduce the chemical substance of complexity in activated carbon, cause the later stage
Difficulty increase is purified, simultaneously because reagent recycling is difficult, brings environmental pollution, it is therefore desirable to effectively improved.
The content of the invention
The purpose of the present invention is to solve product activation effect of the prior art is bad, product quality is bad, the later stage
The defects of purifying difficulty increase, and a kind of production method of the biological activated carbon proposed.
To achieve these goals, present invention employs following technical solution:
The invention discloses a kind of production method of biological activated carbon, comprise the following steps that:
(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;
(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;
(3), under conditions of 200 DEG C by plant fiber drying to moisture 20% within;
(4), under conditions of 400 ~ 600 °C, fibrous raw material is carbonized, carbonization time is 10 ~ 30min, is carbonized
Thing;
(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 700 ~ 900 DEG C, work
The change time is 30 ~ 120min;
(6), adopt that to be washed with deionized to pH value be 5 ~ 7, dry 3-10min, is cooled to room temperature, obtains under the conditions of 200 DEG C
Product.
Preferably, the step(1)In, the plant fiber material is using hardwood, cork, shrub, grass family
In one or more arbitrary proportions combination, the hardwood is using a kind of in Eucalyptus or poplar or at least two
Mixture, the shrub are described using salix monogolica, rose stalk, cuckoo stalk, a kind of in barberry or at least two mixture
Cork use pine, the grass family is using bamboo, straw, wheat straw, cornstalk, reed, one kind in bagasse or extremely
Mixture two kinds few.
Preferably, the step(1)In, the boiling solvent is using in formic acid, acetic acid, n-butyric acie, isobutyric acid
One or more arbitrary proportions combination.
Preferably, the step(1)In, the catalyst is using inorganic acid, one kind in hydrogen peroxide or two
The combination of the arbitrary proportion of person, the quality of the catalyst are the 0.01 ~ 10% of the quality of over dry plant fiber material.
Preferably, the step(1)In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 70 ~ 200
DEG C, the time of boiling is 10 ~ 600min.
Preferably, the step(1)In, the temperature of the boiling is 90 ~ 150 DEG C.
Preferably, the step(1)In, the time of boiling is 50 ~ 300min.
Preferably, the step(2)In, it is 3 ~ 6.5 that plant fiber, which is washed to pH value,.
Preferably, the step(2)In, isolated liquid can be evaporated recycling and make reagent, and can be by it
In hemicellulose and lignin extraction as accessory substance.
Preferably, the step(5)In, the mass ratio of the activator and fiber is 1:1~6:1.
Preferably, the step(5)In, the activator uses KOH.
Compared with prior art, the present invention provides a kind of production method of biological activated carbon, possesses following beneficial effect:
1st, step is passed through(1)Processing, most of hemicellulose is dissolved into liquid system in fibrous raw material, no longer to next
The activation of step causes to suppress, and the influence to activation effect substantially reduces;
2nd, step is passed through(2)Processing, the complex cross-linked structure of lignin and cellulose is broken in fibrous raw material, most of wood
Quality separates out inside fibrous raw material, wherein, it is partly into solution system, meanwhile, another part adheres to after separating out
In fiber extexine, " compound " of cellulose and lignin is formd, this is a kind of special attachment form, such a compound
Due to the presence of lignin, during for producing activated carbon, the yield of activated carbon can be considerably increased, simultaneously as lignin is
Complex cross-linked structure no longer is formed with cellulose, so the activated carbon thus produced has very big specific surface area, adsorption capacity
By force;
3rd, the pretreating reagent that the method is used is organic acid, and utilization, method can be all recycled by way of evaporation and concentration
Environmental protection, cost are low;
4th, KOH is added as activator, and K ions therein contribute to the quick progress that catalytic activation reacts so that the production time
It is short, but be in this method using the method for KOH with the different point of conventional method, in this method step(2)In, fiber wash
Faintly acid is still kept afterwards, on the one hand reduces slurry, on the other hand, the KOH added in subsequent activation can be just to weak acid
Property fiber play partial neutralisation, be that the washing of fiber further reduces pressure after subsequent activation.
Brief description of the drawings
Fig. 1 is a kind of flow chart of the production method of biological activated carbon proposed by the present invention.
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.
In the description of the present invention, it is to be understood that term " on ", " under ", "front", "rear", "left", "right",
The orientation or position relationship of the instruction such as " top ", " bottom ", " interior ", " outer " are based on orientation shown in the drawings or position relationship, are only
Described for the ease of description is of the invention with simplified, rather than the device or element of instruction or hint meaning must be with specifically sides
Position, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.
With reference to Fig. 1, the invention discloses a kind of production method of biological activated carbon, comprise the following steps that:
(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;
(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;
(3), under conditions of 200 DEG C by plant fiber drying to moisture 20% within;
(4), under conditions of 400 ~ 600 °C, fibrous raw material is carbonized, carbonization time is 10 ~ 30min, is carbonized
Thing;
(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 700 ~ 900 DEG C, work
The change time is 30 ~ 120min;
(6), adopt that to be washed with deionized to pH value be 5 ~ 7, dry 3-10min, is cooled to room temperature, obtains under the conditions of 200 DEG C
Product.
Preferably, the step(1)In, the boiling solvent is using in formic acid, acetic acid, n-butyric acie, isobutyric acid
One or more arbitrary proportions combination.
Preferably, the step(1)In, the catalyst is using inorganic acid, one kind in hydrogen peroxide or two
The combination of the arbitrary proportion of person, the quality of the catalyst are the 0.01 ~ 10% of the quality of over dry plant fiber material.
Preferably, the step(1)In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 70 ~ 200
DEG C, the time of boiling is 10 ~ 600min.
Preferably, the step(1)In, the plant fiber material is using hardwood, cork, shrub, grass family
In one or more arbitrary proportions combination, the hardwood is using a kind of in Eucalyptus or poplar or at least two
Mixture, the shrub are described using salix monogolica, rose stalk, cuckoo stalk, a kind of in barberry or at least two mixture
Cork use pine, the grass family is using bamboo, straw, wheat straw, cornstalk, reed, one kind in bagasse or extremely
Mixture two kinds few.
Preferably, the step(1)In, the temperature of the boiling is 90 ~ 150 DEG C.
Preferably, the step(1)In, the time of boiling is 50 ~ 300min.
Preferably, the step(2)In, it is 3 ~ 6.5 that plant fiber, which is washed to pH value,.
Preferably, the step(2)In, isolated liquid can be evaporated recycling and make reagent, and can be by it
In hemicellulose and lignin extraction as accessory substance.
Preferably, the step(5)In, the mass ratio of the activator and fiber is 1:1~6:1.
Preferably, the step(5)In, the activator uses KOH.
Embodiment 1
The invention discloses a kind of production method of biological activated carbon, comprise the following steps that:
(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;
(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;
(3), under conditions of 200 DEG C by plant fiber drying to moisture 18%;
(4), under conditions of 500 °C, fibrous raw material is carbonized, carbonization time 15min, obtain carbide;
(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 800 DEG C, during activation
Between be 75min;
(6), adopt that to be washed with deionized to pH value be 6, dry 7min, is cooled to room temperature, obtains product under the conditions of 200 DEG C.
The step(1)In, the plant fiber material uses Eucalyptus.
The step(1)In, the boiling solvent uses formic acid.
The step(1)In, the catalyst uses inorganic acid, and the quality of the catalyst is over dry plant fiber
The 5% of the quality of raw material.
The step(1)In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 180 DEG C, the time of boiling
For 400min.
The step(2)In, it is 5 that plant fiber, which is washed to pH value,.
The step(2)In, isolated liquid can be evaporated recycling and make reagent, and can be by hemicellulose therein
Element is with lignin extraction as accessory substance.
The step(5)In, the mass ratio of the activator and fiber is 1:1.
The step(5)In, the activator uses KOH.
Embodiment 2
The invention discloses a kind of production method of biological activated carbon, comprise the following steps that:
(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;
(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;
(3), under conditions of 200 DEG C by plant fiber drying to moisture 16%;
(4), under conditions of 600 °C, fibrous raw material is carbonized, carbonization time 30min, obtain carbide;
(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 700 DEG C, during activation
Between be 120min;
(6), adopt that to be washed with deionized to pH value be 5, dry 10min, is cooled to room temperature, obtains product under the conditions of 200 DEG C.
The step(1)In, the plant fiber material uses bagasse.
The step(1)In, the boiling solvent uses acetic acid.
The step(1)In, the catalyst uses hydrogen peroxide, and the quality of the catalyst is over dry plant fibre
Tie up the 0.01% of the quality of raw material.
The step(1)In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 70 DEG C, the time of boiling
For 600min.
The step(2)In, it is 6.5 that plant fiber, which is washed to pH value,.
The step(2)In, isolated liquid can be evaporated recycling and make reagent, and can be by hemicellulose therein
Element is with lignin extraction as accessory substance.
The step(5)In, the mass ratio of the activator and fiber is 3:1.
The step(5)In, the activator uses KOH.
Embodiment 3
The invention discloses a kind of production method of biological activated carbon, comprise the following steps that:
(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;
(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;
(3), under conditions of 200 DEG C by plant fiber drying to moisture 17%;
(4), under conditions of 420 °C, fibrous raw material is carbonized, carbonization time 13min, obtain carbide;
(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 750 DEG C, during activation
Between be 59min;
(6), adopt that to be washed with deionized to pH value be 7, dry 3min, is cooled to room temperature, obtains product under the conditions of 200 DEG C.
The step(1)In, the plant fiber material uses wheat straw.
The step(1)In, the boiling solvent uses n-butyric acie.
The step(1)In, the catalyst uses hydrogen peroxide, and the quality of the catalyst is over dry plant fibre
Tie up the 0.09% of the quality of raw material.
The step(1)In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 99 DEG C, the time of boiling
For 500min.
The step(2)In, it is 4.5 that plant fiber, which is washed to pH value,.
The step(2)In, isolated liquid can be evaporated recycling and make reagent, and can be by hemicellulose therein
Element is with lignin extraction as accessory substance.
The step(5)In, the mass ratio of the activator and fiber is 3:1.
The step(5)In, the activator uses KOH.
Embodiment 4
The invention discloses a kind of production method of biological activated carbon, comprise the following steps that:
(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;
(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;
(3), under conditions of 200 DEG C by plant fiber drying to moisture 17%;
(4), under conditions of 600 °C, fibrous raw material is carbonized, carbonization time 10min, obtain carbide;
(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 900 DEG C, during activation
Between be 120min;
(6), adopt that to be washed with deionized to pH value be 5, dry 10min, is cooled to room temperature, obtains product under the conditions of 200 DEG C.
The step(1)In, the plant fiber material uses reed.
The step(1)In, the boiling solvent uses isobutyric acid.
The step(1)In, the catalyst uses inorganic acid, and the quality of the catalyst is over dry plant fiber
The 7% of the quality of raw material.
The step(1)In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 180 DEG C, the time of boiling
For 200min.
The step(2)In, it is 6.5 that plant fiber, which is washed to pH value,.
The step(2)In, isolated liquid can be evaporated recycling and make reagent, and can be by hemicellulose therein
Element is with lignin extraction as accessory substance.
The step(5)In, the mass ratio of the activator and fiber is 4:1.
The step(5)In, the activator uses KOH.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
- A kind of 1. production method of biological activated carbon, it is characterised in that:Comprise the following steps that:(1), catalyst is added into boiling solvent, and add plant fiber material carry out boiling processing;(2), carry out separation of solid and liquid after the completion of boiling, the plant fiber after being handled, plant fiber is washed to faintly acid;(3), under conditions of 200 DEG C by plant fiber drying to moisture 20% within;(4), under conditions of 400 ~ 600 °C, fibrous raw material is carbonized, carbonization time is 10 ~ 30min, is carbonized Thing;(5), add activator, activator is mixed and crushed with carbide, is activated under conditions of 700 ~ 900 DEG C, work The change time is 30 ~ 120min;(6), adopt that to be washed with deionized to pH value be 5 ~ 7, dry 3-10min, is cooled to room temperature, obtains under the conditions of 200 DEG C Product.
- A kind of 2. production method of biological activated carbon according to claim 1, it is characterised in that:The step(1)In, The boiling solvent using formic acid, acetic acid, n-butyric acie, one or more arbitrary proportions in isobutyric acid combination.
- A kind of 3. production method of biological activated carbon according to claim 1 or 2, it is characterised in that:The step(1) In, the catalyst using inorganic acid, the arbitrary proportion of one or both in hydrogen peroxide combination, the catalyst Quality is the 0.01 ~ 10% of the quality of over dry plant fiber material.
- A kind of 4. production method of biological activated carbon according to claim 1 or 2, it is characterised in that:The step(1) In, the pressure of boiling is atmospheric cooking, and the temperature of the boiling is 70 ~ 200 DEG C, and the time of boiling is 10 ~ 600min.
- A kind of 5. production method of biological activated carbon according to claim 1 or 2, it is characterised in that:The step(1) In, the temperature of the boiling is 90 ~ 150 DEG C, and the time of boiling is 50 ~ 300min.
- A kind of 6. production method of biological activated carbon according to claim 1, it is characterised in that:The step(1)In, The plant fiber material is using the combination of hardwood, cork, shrub, one or more arbitrary proportions in grass family, institute The hardwood stated using a kind of in Eucalyptus or poplar or at least two mixture, the shrub using salix monogolica, rose stalk, A kind of in cuckoo stalk, barberry or at least two mixture, the cork use pine, and the grass family uses A kind of in bamboo, straw, wheat straw, cornstalk, reed, bagasse or at least two mixture.
- A kind of 7. production method of biological activated carbon according to claim 1, it is characterised in that:The step(2)In, It is 3 ~ 6.5 that plant fiber, which is washed to pH value,.
- A kind of 8. production method of biological activated carbon according to claim 1 or 7, it is characterised in that:The step(2) In, isolated liquid can be evaporated recycling and make reagent, and can be using hemicellulose therein and lignin extraction as pair Product.
- A kind of 9. production method of biological activated carbon according to claim 1, it is characterised in that:The step(5)In, The activator and the mass ratio of fiber are 1:1~6:1.
- A kind of 10. production method of biological activated carbon according to claim 1 or 9, it is characterised in that:The step (5)In, the activator uses KOH.
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CN111232978A (en) * | 2020-03-26 | 2020-06-05 | 南京林业大学 | Method for preparing high-yield activated carbon by grouping and separating shell biomass |
CN115974744A (en) * | 2022-12-27 | 2023-04-18 | 晨光生物科技集团股份有限公司 | Production method and application of marigold extract |
CN116262875A (en) * | 2021-12-13 | 2023-06-16 | 中国石油化工股份有限公司 | Efficient plugging agent for drilling fluid and preparation method and application thereof |
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