CN106975449A - A kind of preparation method and applications of celery charcoal - Google Patents
A kind of preparation method and applications of celery charcoal Download PDFInfo
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- CN106975449A CN106975449A CN201710323843.9A CN201710323843A CN106975449A CN 106975449 A CN106975449 A CN 106975449A CN 201710323843 A CN201710323843 A CN 201710323843A CN 106975449 A CN106975449 A CN 106975449A
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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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
- 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
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
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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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses a kind of preparation method and applications of celery charcoal, its preparation method comprises the following steps：Material activating：Celery after drying is positioned in weak acid solution and soaked, it is shaken, filter, rinsed, it is standby；Drying and crushing：Material is dried again to constant weight, then standby material is crushed, sieved for subsequent use；The preparation of charcoal：Material is positioned over after being heated in crucible and be cooled to after room temperature; first it is placed in Muffle furnace logical nitrogen to protect it, leads to nitrogen protection in Muffle furnace afterwards and carbonized, cooled down; material mixing after charing is uniformly ground, sieve, preserved, celery charcoal is made；Present invention simultaneously relates to application of the celery charcoal in absorption bisphenol-A solution.Celery charcoal prepared by the present invention is to bisphenol-A high adsorption capacity, and stability is high, realizes the utilization of agricultural wastes recycling, and provide a kind of easily mode to improve water quality.
Description
Technical field
The invention belongs to water-treatment technology field, more particularly to a kind of preparation method and applications of celery charcoal.
Background technology
Bisphenol-A (bisphenol A, BPA), industrially to be used to polycarbonate synthesis and epoxy resin etc. more for bisphenol-A
High polymer material is planted, production mineral water bottle, medicine equipment and packaging for foodstuff are widely used in plastic products inside.BPA quilts
Report has female hormone activity, is a kind of incretion interferent, can also cause animal to produce female even if very low dosage early
The effects such as ripe, sperm count declines, prostate growth.In addition, it also has certain embryotoxicity and teratogenesis, can substantially it increase
The generation of the cancers such as animal ovary cancer, prostate cancer, leukaemia.Substantially detection has in the source quality detection of current China
BPA, therefore remove focus of the method as research of BPA in water environment.
Charcoal carbonizes formation under anoxic conditions using biomass, because of its stronger adsorption capacity and ambient stable
Property and attract attention.Charcoal has certain suction-operated to organic pollution, heavy metal ion etc..According to incompletely statistics,
Vegetable waste discharge capacity is more than 2,000,000,000 tons in the annual agricultural production of China, part agricultural wastes tradition as compost,
Feed, the primary raw material for producing biogas.Charcoal is prepared by raw material of abandoned vegetable, it is new by one as its recycling
Approach.
Celery charcoal of the present invention, can not only realize agricultural wastes recycling, simple and easy to apply, and can profit
The developing of new product can be carried out with its unique purposes.
The content of the invention
It is an object of the invention to effectively be used without edibility or discarded agricultural wastes, using celery as raw material system
The standby improvement charcoal for obtaining super quality and competitive price, is further used for improving water quality.
To overcome deficiency of the prior art, the present invention provides a kind of solution of the preparation method and applications of celery charcoal
Certainly scheme, specific as follows：
A kind of preparation method of celery charcoal, comprises the following steps：
Step 1.1 material activating：By the celery drying after cleaning, material is positioned in weak acid solution again after drying and soaked
Bubble, is put into oscillator closed concussion by mixed material, it is filtered, rinsed to neutrality, standby；
Step 1.2 drying and crushing：Material in step 1.1 is dried to constant weight, then by the crushing of standby material, mistake again
Sieve, it is standby；
The preparation of step 1.3 charcoal：Material in step 1.2 is positioned in crucible, will untill being heated to not smoldering
It is cooled to after room temperature, is first placed in Muffle furnace logical nitrogen at room temperature and it is protected, afterwards in Muffle furnace
Logical nitrogen protection is carbonized, and is taken out, is put into glass capsulation tank and is cooled to room temperature, the material mixing after charing is uniformly carried out
After grinding, sieving, store in drier, celery charcoal is made.
It is preferred that, step 1.1 is specially：Using celery discarded or without edibility, its surface attachment is cleaned
After thing, celery is cut into 1~3cm section shape, 4~6h of drying under 60 DEG C~100 DEG C environment is then placed within, again by west after drying
Celery, which is positioned in the weak acid solution that concentration is 20%~40%, to be soaked, wherein, dry celery presses 5~15g/ with weak acid solution
100ml ratio mixing, mixed material is put into oscillator after 6~10h of closed concussion, rushed after filtering with deionized water
Neutrality is washed till, it is standby.
It is preferred that, step 1.2 is specially：Material in step 1.1 is put into the environment of 90~120 DEG C and dried to perseverance
Weight, after then standby substance migration electric crusher is crushed, crosses 80 mesh sieves, standby.
It is preferred that, step 1.3 is specially：Material in step 1.2 is positioned in crucible, untill being heated to not smoldering,
It is cooled to after room temperature, is first placed in Muffle furnace logical nitrogen at room temperature and 0.5~1.5h of protection is carried out to it, afterwards
Lead to nitrogen protection in reaction temperature is 200~500 DEG C of Muffle furnaces and carry out 2~4h of charing, take out, be put into cold in glass capsulation tank
But to room temperature, after the material mixing after charing is uniformly ground, sieved, store in drier, celery charcoal is made.
It is preferred that, in step 1.1, the weak acid solution is in oxalic acid solution, acetum or hydrogenperoxide steam generator
It is a kind of.
It is preferred that, the flow for leading to nitrogen is 200ml/min, and heating rate is 10~20 DEG C/min.
It is preferred that, in step 1.3, sieve as 100 mesh sieves, sieving gained as celery charcoal.
The present invention also protects the celery charcoal to apply in water treatment procedure simultaneously.
It is preferred that, it is specifically the application in absorption bisphenol-A solution.
It is preferred that, the application is specially：The celery charcoal is molten by 5g/l dosage addition 100ng/ml bisphenol-As
In liquid, after being fully vortexed, then it is centrifuged 5~10min by 5000rmp of rotating speed, takes supernatant by 10~20min of standing adsorption
Liquid carries out LC Mass.
Beneficial effects of the present invention are：Using it is a kind of without edibility or discarded celery to be used as raw material to prepare biological
Charcoal, raw material sources are conveniently easy to get, and the recycling of discarded object is also achieved while celery charcoal is prepared；Celery fiber
Cellulose content is high, and the charcoal absorption property of preparation is good；In celery charcoal preparation process it is pollution-free and prepare it is simple, by grass
Acid activation, absorption property is further enhanced, short preparation period, with application value.
Brief description of the drawings
Fig. 1 is the process chart for preparing celery charcoal.
Embodiment
The content of the invention is described further with reference to the accompanying drawings and examples：
Embodiment 1：
A kind of preparation method of celery charcoal, comprises the following steps：
Step 1.1 material activating：Using celery discarded or without edibility, clean after its surface attachments,
Celery is cut into 1cm section shape, is then placed within 60 DEG C of environment and dries 6h, it is 20% that celery is positioned over into concentration again after drying
Acetum in soak, wherein, dry celery and ratio mixing of the acetum in 5g/100ml, by mixed material
It is put into oscillator after closed concussion 10h, it is standby with deionized water rinsing to neutrality after filtering.
Step 1.2 drying and crushing：Material in step 1.1 is put into the environment of 90 DEG C and dried to constant weight, then will be standby
After being crushed with substance migration electric crusher, 80 mesh sieves are crossed, it is standby；
The preparation of step 1.3 charcoal：Material in step 1.2 is positioned in crucible, will untill being heated to not smoldering
It is cooled to after room temperature, is first placed in Muffle furnace logical nitrogen at room temperature and is carried out protection 0.5h to it, afterwards in reaction
Temperature carries out charing 4h to lead to nitrogen protection in 200 DEG C of Muffle furnace, and the flow for leading to nitrogen is 200ml/min, and heating rate is
10℃/min.Take out, be put into glass capsulation tank and be cooled to room temperature, the material mixing after charing is uniformly ground, cross 100
After mesh sieve, store in drier, celery charcoal XQ-1 is made.
The present invention also protects the celery charcoal to apply in water treatment procedure simultaneously.It is specifically molten in absorption bisphenol-A
Application in liquid.Specifically, XQ-1 is added in 100ng/ml BPA solution by 5g/l dosage, after being fully vortexed, stand and inhale
Attached 10min, then centrifuges 5min by 5000rmp of rotating speed by it, then takes supernatant to carry out LC Mass test,
Obtain the test result of table 1：
Table 1
| Product title | Reaction temperature/DEG C | Yield/% | BPA clearances/% |
| XQ-1 | 200 | 20.21 | 80 |
Embodiment 2：
A kind of preparation method of celery charcoal, comprises the following steps：
Step 1.1 material activating：Using celery discarded or without edibility, clean after its surface attachments,
Celery is cut into 2cm section shape, is then placed within 80 DEG C of environment and dries 5h, it is 30% that celery is positioned over into concentration again after drying
Hydrogenperoxide steam generator in soak, wherein, dry celery and ratio mixing of the hydrogenperoxide steam generator by 10g/100ml will be mixed
Material after conjunction is put into oscillator after closed concussion 8h, standby with deionized water rinsing to neutrality after filtering.
Step 1.2 drying and crushing：Material in step 1.1 is put into the environment of 100 DEG C and dried to constant weight, then will be standby
After being crushed with substance migration electric crusher, 80 mesh sieves are crossed, it is standby；
The preparation of step 1.3 charcoal：Material in step 1.2 is positioned in crucible, will untill being heated to not smoldering
It is cooled to after room temperature, is first placed in Muffle furnace logical nitrogen at room temperature and is carried out protection 1h to it, afterwards in reaction temperature
Spend in the Muffle furnace for 300 DEG C and be connected with nitrogen protection progress charing 2h, the flow for leading to nitrogen is 200ml/min, and heating rate is
20℃/min.Take out, be put into glass capsulation tank and be cooled to room temperature, the material mixing after charing is uniformly ground, cross 100
After mesh sieve, store in drier, celery charcoal XQ-2 is made.
The present invention also protects the celery charcoal to apply in water treatment procedure simultaneously.It is specifically molten in absorption bisphenol-A
Application in liquid.Specifically, XQ-2 is added in 100ng/ml BPA solution by 5g/l dosage, after being fully vortexed, stand and inhale
Attached 15min, then centrifuges 8min by 5000rmp of rotating speed by it, then takes supernatant to carry out LC Mass test,
Obtain the test result of table 2：
Table 2
| Product title | Reaction temperature/DEG C | Yield/% | BPA clearances/% |
| XQ-2 | 300 | 22.46 | 73 |
Embodiment 3：
A kind of preparation method of celery charcoal, comprises the following steps：
Step 1.1 material activating：Using celery discarded or without edibility, clean after its surface attachments,
Celery is cut into 3cm section shape, is then placed within 100 DEG C of environment and dries 4h, celery is positioned over into concentration again after drying is
Soaked in 40% oxalic acid solution, wherein, dry celery and oxalic acid solution is mixed in 15g/100ml ratio, after mixing
Material be put into oscillator after closed concussion 6h, it is standby with deionized water rinsing to neutrality after filtering.
Step 1.2 drying and crushing：Material in step 1.1 is put into the environment of 120 DEG C and dried to constant weight, then will be standby
After being crushed with substance migration electric crusher, 80 mesh sieves are crossed, it is standby；
The preparation of step 1.3 charcoal：Material in step 1.2 is positioned in crucible, will untill being heated to not smoldering
It is cooled to after room temperature, is first placed in Muffle furnace logical nitrogen at room temperature and is carried out protection 1.5h to it, afterwards in reaction
Temperature carries out charing 3h to lead to nitrogen protection in 400 DEG C of Muffle furnace, and the flow for leading to nitrogen is 200ml/min, and heating rate is
15℃/min.Take out, be put into glass capsulation tank and be cooled to room temperature, the material mixing after charing is uniformly ground, cross 100
After mesh sieve, store in drier, celery charcoal XQ-3 is made.
The present invention also protects the celery charcoal to apply in water treatment procedure simultaneously.It is specifically molten in absorption bisphenol-A
Application in liquid.Specifically, XQ-3 is added in 100ng/ml BPA solution by 5g/l dosage, after being fully vortexed, stand and inhale
Attached 20min, then centrifuges 10min by 5000rmp of rotating speed by it, then takes supernatant to carry out LC Mass survey
Examination, obtains the test result of table 1：
Table 3
| Product title | Reaction temperature/DEG C | Yield/% | BPA clearances/% |
| XQ-3 | 400 | 25.37 | 82 |
Embodiment 4：
A kind of preparation method of celery charcoal, comprises the following steps：
Step 1.1 material activating：Using celery discarded or without edibility, clean after its surface attachments,
Celery is cut into 2cm section shape, is then placed within 80 DEG C of environment and dries 5h, it is 30% that celery is positioned over into concentration again after drying
Oxalic acid solution in soak, wherein, dry celery and ratio mixing of the oxalic acid solution in 10g/100ml, by mixed thing
Matter is put into oscillator after closed concussion 8h, standby with deionized water rinsing to neutrality after filtering.
Step 1.2 drying and crushing：Material in step 1.1 is put into the environment of 105 DEG C and dried to constant weight, then will be standby
After being crushed with substance migration electric crusher, 80 mesh sieves are crossed, it is standby；
The preparation of step 1.3 charcoal：Material in step 1.2 is positioned in crucible, will untill being heated to not smoldering
It is cooled to after room temperature, is first placed in Muffle furnace logical nitrogen at room temperature and is carried out protection 1h to it, afterwards in reaction temperature
Spend in the Muffle furnace for 500 DEG C and lead to nitrogen protection progress charing 3h, the flow for leading to nitrogen is 200ml/min, and heating rate is 10
℃/min.Take out, be put into glass capsulation tank and be cooled to room temperature, the material mixing after charing is uniformly ground, cross 100 mesh
After sieve, store in drier, celery charcoal XQ-4 is made.
The present invention also protects the celery charcoal to apply in water treatment procedure simultaneously.It is specifically molten in absorption bisphenol-A
Application in liquid.Specifically, XQ-4 is added in 100ng/ml BPA solution by 5g/l dosage, after being fully vortexed, stand and inhale
Attached 10min, then centrifuges 5min by 5000rmp of rotating speed by it, then takes supernatant to carry out LC Mass test,
Obtain the test result of table 1：
Table 4
| Product title | Reaction temperature/DEG C | Yield/% | BPA clearances/% |
| XQ-4 | 500 | 50.23 | 94 |
In addition, compared with pomelo peel charcoal prepared by same method, showing the suction of celery charcoal by test result
Attached performance is more preferable.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as be without departing from technical solution of the present invention content, according to the technical spirit of the present invention,
Within the spirit and principles in the present invention, any simple modification, equivalent substitution and improvement for being made to above example etc., still
Belong within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of preparation method of celery charcoal, it is characterised in that comprise the following steps：
Step 1.1 material activating：By the celery drying after cleaning, material is positioned in weak acid solution again after drying and soaked, will
Mixed material is put into oscillator closed concussion, and it is filtered, rinsed to neutrality, standby；
Step 1.2 drying and crushing：Material in step 1.1 is dried to constant weight again, then standby material is crushed, sieved,
It is standby；
The preparation of step 1.3 charcoal：Material in step 1.2 is positioned in crucible, it is untill being heated to not smoldering, its is cold
But it is protected to after room temperature, being first placed in Muffle furnace leading to nitrogen at room temperature, leads to nitrogen in Muffle furnace afterwards
Gas shielded is carbonized, and is taken out, is put into glass capsulation tank and is cooled to room temperature, the material mixing after charing is uniformly ground
After mill, sieving, store in drier, celery charcoal is made.
2. a kind of preparation method of celery charcoal according to claim 1, it is characterised in that step 1.1 is specially：Adopt
With celery discarded or without edibility, clean after its surface attachments, celery is cut into 1~3cm section shape, then
4~6h of drying is placed under 60 DEG C~100 DEG C environment, it is molten that celery is positioned over into the weak acid that concentration is 20%~40% again after drying
Soaked in liquid, wherein, dry celery and weak acid solution is mixed in 5~15g/100ml ratio, and mixed material is put into
It is standby with deionized water rinsing to neutrality after filtering in oscillator after 6~10h of closed concussion.
3. a kind of preparation method of celery charcoal according to claim 1, it is characterised in that step 1.2 is specially：Will
Material in step 1.1 is dried in the environment of being put into 90~120 DEG C to constant weight, is then entered standby substance migration electric crusher
After row is crushed, 80 mesh sieves are crossed, it is standby.
4. a kind of preparation method of celery charcoal according to claim 1, it is characterised in that step 1.3 is specially：Will
Material in step 1.2 is positioned in crucible, untill being heated to not smoldering, is cooled to after room temperature, is first placed on horse
Not lead to nitrogen in stove at room temperature and 0.5~1.5h of protection is carried out to it, afterwards in reaction temperature is 200~500 DEG C of Muffle furnaces
Logical nitrogen protection carries out 2~4h of charing, takes out, is put into glass capsulation tank and is cooled to room temperature, and the material mixing after charing is equal
It is even be ground, sieve after, store in drier, celery charcoal be made.
5. the preparation method of a kind of celery charcoal according to claim 1 or 2, it is characterised in that in step 1.1,
The weak acid solution is one kind in oxalic acid solution, acetum or hydrogenperoxide steam generator.
6. according to claim 1, a kind of preparation method of celery charcoal described in any one of 2,3 or 4, its feature exists
In the flow for leading to nitrogen is 200ml/min, and heating rate is 10~20 DEG C/min.
7. the preparation method of a kind of celery charcoal according to claim 1, it is characterised in that in step 1.3, sieving
For 100 mesh sieves, sieving gained is celery charcoal.
8. by claim 1, celery charcoal is applied in water treatment procedure any one of 2,3,4,7.
9. application according to claim 8, it is characterised in that be specifically the application in absorption bisphenol-A solution.
10. application according to claim 9, it is characterised in that the application is specially：The celery charcoal is pressed
5g/l dosage is added in 100ng/ml bisphenol-A solution, after being fully vortexed, 10~20min of standing adsorption, then by it with rotating speed
5~10min is centrifuged for 5000rmp, takes supernatant to carry out LC Mass.
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| CN108435135A (en) * | 2018-05-25 | 2018-08-24 | 广州大学 | A kind of preparation method of watermelon peel charcoal and its in removing waste water thallium application |
| CN109111936A (en) * | 2018-08-01 | 2019-01-01 | 湖南工业大学 | A kind of charcoal and preparation method thereof of evaporation processing in situ |
| CN109173994A (en) * | 2018-09-19 | 2019-01-11 | 南昌航空大学 | A kind of modified abandoned stub of high temperature carbonization prepares the method for charcoal and the application of charcoal |
| CN109879696A (en) * | 2019-04-02 | 2019-06-14 | 郭光光 | Biological carbon base compound fertilizer and preparation method thereof |
| CN113620370A (en) * | 2021-10-14 | 2021-11-09 | 生态环境部华南环境科学研究所 | Method for efficiently removing bisphenol pollutants in water body and compound biochar material |
| CN113620370B (en) * | 2021-10-14 | 2021-12-17 | 生态环境部华南环境科学研究所 | Method for efficiently removing bisphenol pollutants in water body and compound biochar material |
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