CN110193348A - A kind of preparation method and applications of nitrogen P Modification lotus leaf charcoal - Google Patents
A kind of preparation method and applications of nitrogen P Modification lotus leaf charcoal Download PDFInfo
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- CN110193348A CN110193348A CN201910513030.5A CN201910513030A CN110193348A CN 110193348 A CN110193348 A CN 110193348A CN 201910513030 A CN201910513030 A CN 201910513030A CN 110193348 A CN110193348 A CN 110193348A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—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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- 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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- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a kind of preparation method and applications of nitrogen P Modification lotus leaf charcoal.Preparation method of the invention includes that the cleaning of lotus leaf is dried and pulverized and sieved, the ammonium dibasic phosphate solution ultrasonic treatment of Lotus Leaf, the pyrolysis charring of modified Lotus Leaf and etc..Resulting materials of the present invention, enable to lotus leaf charcoal that there are more adsorption sites, enhance lotus leaf charcoal absorption property, realize the recycling of agriculture and forestry organic waste material simultaneously, the effect efficiently administered can also be played in heavy metal environmental pollution, and processing cost is low, and environmentally friendly, will not bring secondary pollution.
Description
Technical field
The present invention relates to environment functional materials, are related to a kind of preparation method and applications of nitrogen P Modification lotus leaf charcoal.
Background technique
Heavy metal pollution is one kind of environmental pollution, due to its toxicity, not biodegradable property and natural and
Being widely present in the environment artificially changed, constitutes a serious threat to environment and the mankind, people for heavy metal pollution more
Concern.Heavy metal is generally widely present in nature, but since the mankind make the exploitation of heavy metal, smelting, processing and business
The activity of making is increasing, and many heavy metals such as lead, mercury, cadmium, cobalt is caused to enter big gas and water, in soil, cause serious environment
Pollution.With heavy metal existing for various chemical states or chemical form, it will retain, accumulate after entering environment or the ecosystem
And migration, it causes damages.It there is now processing of the various technologies for heavy metal, including precipitating, ion exchange, absorption, film
Filtering, reverse osmosis, evaporation recycling, coagulation, solvent extraction, reduction electrolysis etc..Wherein, absorption is as a kind of easy to operate, cost
It is cheap, and the higher technology for the treatment of effeciency has application in actual waste water improvement.
Charcoal is a kind of solid that height aromatization is hard to tolerate that biomass is generated through pyrolysis carbonization under anoxic conditions
Matter broadly belongs to one kind of black wood charcoal.Charcoal contains the micropore and nano-pore of a large amount of aromatic structure, makes it for heavy metal
Or other pollutants have stronger adsorption capacity.However, shadow of the property of charcoal by its raw material and pyrolytical condition
Sound is very big, and the adsorption site that non-modified or functional modification charcoal has is very limited, to limit it in reality
Application in wastewater treatment.Therefore, charcoal is effectively modified, to obtain preferable application, is had extremely important
Meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of at low cost, removal effect it is good can be used for adsorption treatment heavy metal contaminants
Nitrogen P Modification lotus leaf charcoal preparation method and applications.
The technical solution of the present invention is as follows:
A kind of preparation method of nitrogen P Modification lotus leaf charcoal carries out at functionalization charcoal through diammonium hydrogen phosphate and ultrasound
Reason, so that abundant phosphate group, hydroxyl group and amino group are assembled in biological carbon surface, these group energy and metal ion
Stable chelate is formed, while also significantly improving the specific surface area of charcoal, increases the adsorption site quantity of biological carbon surface,
Charcoal is improved to the removal ability of heavy metal, is specifically comprised the following steps:
(1) biomass raw material lotus leaf is cleaned with deionized water, lotus leaf is placed in pulverizer after drying and crushes and is sieved；
(2) ammonium dibasic phosphate solution is prepared；
(3) solid-liquid mass ratio for pressing 1:15 ~ 25, weigh Lotus Leaf obtained by step (1) be added into step (2) acquired solution it is super
It sound 3 ~ 5 hours, then dries and grinds, obtain modified Lotus Leaf；
(4) modified Lotus Leaf obtained by step (3) is put into the pyrolysis carried out in tube furnace under anoxia condition to fire, fires and completes
After be cooled to room temperature after take out；
(5) by the charcoal of taking-up with milli-Q water several times until washing lotion pH value do not change, dry again, obtain nitrogen phosphorus and change
The lotus leaf charcoal of property.
Further, in step (1), drying temperature is 70 ~ 110 DEG C, and drying time is 18 ~ 30 hours.
Further, in step (1), the sieve of 100 ~ 300 mesh is selected in sieving.
Further, in step (2), ultrapure water is added in volumetric flask by weighing diammonium hydrogen phosphate in ammonium dibasic phosphate solution
It is settled to scale to obtain, the concentration of ammonium dibasic phosphate solution is 0.3 ~ 1 mol/L.
Further, in step (4), pyrolysis temperature is 400 ~ 600 DEG C, and the close of tube furnace quartz ampoule is kept in pyrolytic process
Feng Xing, while N is passed through with the air-flow velocity of 30 ~ 60mL/min2, it is ensured that the anoxia condition in whole process quartz ampoule, tube furnace
Temperature program: be heated to 400 ~ 600 DEG C from room temperature, heating rate is 5 ~ 10 DEG C/min, and 400 ~ 600 DEG C of conditions is kept to continue
Pyrolysis 0.8 ~ 1.2 hour, then starts nature and is down to room temperature, to be endlessly passed through N in the whole process2And it keeps
N2Flow velocity it is constant.
Further, in step (5), drying temperature is 70 ~ 100 DEG C.
In above-mentioned preparation method, the raw material selection lotus leaf of charcoal is from a wealth of sources, low in cost, the method for preparation
Simply, easy to operate, easy popularization.
The application of lead ion of the nitrogen P Modification lotus leaf charcoal that above-mentioned preparation method obtains in removal water body.
The specific method of above-mentioned application, comprising the following steps:
Nitrogen P Modification lotus leaf charcoal is mixed with lead waste water, obtains purified solution through concussion, ultrafiltration.
Further, the plumbum ion concentration of the leaded ion waste water is 10 ~ 500mg/L.
Further, the solid-to-liquid ratio of the nitrogen P Modification charcoal and leaded ion waste water is the g/mL of 1:10 ~ 100；That is,
In mass, leaded ion waste water is by volume for nitrogen P Modification lotus leaf charcoal.
Further, the revolving speed of the concussion is 100 ~ 400rpm, and temperature requirement is not high, room temperature, preferably 20 ~ 30
℃。
Compared with prior art, of the invention to be a little:
(1) biological carbon feedstock lotus leaf used in the present invention is from a wealth of sources and cheap, can be realized returning for agriculture and forestry organic waste material
Receive utilization or resource utilization；And diammonium hydrogen phosphate involved in raw material is common chemical products.
(2) simple process of nitrogen P Modification lotus leaf charcoal of the invention, preparation is quick, and technology stability is good.
(3) present invention improves specific surface area and the hole of charcoal by diammonium hydrogen phosphate and supersonic modifying lotus leaf charcoal
Hold, increase adsorption site, improve lotus leaf charcoal for the adsorption capacity of pollutant, while being added on the surface of charcoal
Amino and phosphate group are conducive to heavy metal and complexing occurs for biological carbon surface, hence it is evident that increase charcoal for a huge sum of money
The adsorbance of category.
(4) this product is nontoxic, environmentally friendly.
Detailed description of the invention
Fig. 1 is the infared spectrum of the nitrogen P Modification lotus leaf charcoal in embodiment 1.
Fig. 2 is the BET map of the nitrogen P Modification lotus leaf charcoal in embodiment 1.
Fig. 3 is nitrogen P Modification lotus leaf charcoal in embodiment 2 to the removal effect figure of lead ion.
Specific implementation method
Invention is described in further details below with reference to Figure of description and specific embodiment,
Embodiment 1
The preparation of nitrogen P Modification lotus leaf charcoal, it is specific the preparation method is as follows:
Lotus leaf is cleaned with ultrapure water, is then dried 24 hours at 80 DEG C, the charcoal after drying is put into powder in pulverizer
It is broken, then with the sieve of 100 mesh, it is placed at dry and saves, it is spare.3.9617g phosphoric acid is added in the volumetric flask of 100mL
Hydrogen diammonium is added ultrapure water and is settled to scale, shakes up.It weighs 100 mesh Lotus Leaf 5g below in the balance to be placed in a beaker, add
Enter the ammonium dibasic phosphate solution that 100mL is prepared in advance, beaker is put into ultrasound 4h in ultrasonic cleaning machine, dries, will dry in 80 DEG C
Sample after dry is ground with agate mortar, and sealing is set and saved at dry.Again by the Lotus Leaf after nitrogen P Modification obtained above
It is put into be pyrolyzed in tube furnace and fire, the leakproofness of tube furnace quartz ampoule is kept in pyrolytic process, while with the air-flow of 50mL/min
Flow velocity is passed through N2, it is ensured that the anoxia condition in whole process quartz ampoule, the temperature program of tube furnace: being heated to 600 DEG C from room temperature,
10 DEG C/min of heating rate, and 600 DEG C of conditions is kept persistently to be pyrolyzed 1 hour, then start nature and be down to room temperature, in whole process
In to be endlessly passed through N2And keep N2Flow velocity it is constant, after being cooled to room temperature take out.The charcoal of taking-up is used super
Pure water is put into baking oven 80 DEG C of drying, obtains nitrogen P Modification lotus leaf charcoal for several times until washing lotion pH value does not change.
Nitrogen P Modification lotus leaf charcoal appearance obtained above is in black, and infrared spectrum measurement and BET measurement are carried out to it.
By infrared spectroscopy Fig. 1 of nitrogen P Modification lotus leaf charcoal it is found that in 1100cm-1Place is the stretching vibration peak of P=O key,
3500cm-1Place is the stretching vibration peak of-OH.In 1300cm-1Place is the stretching vibration peak of C-N key.Infrared spectrogram illustrates N, P
It is entrained on charcoal well.It is 34.603m according to the specific surface area of BET map nitrogen P Modification lotus leaf charcoal2/g。
Embodiment 2
The preparation of nitrogen P Modification lotus leaf charcoal, it is specific the preparation method is as follows:
The preparation of (1) the 100 following Lotus Leaf of mesh: lotus leaf is cleaned with ultrapure water, is then dried 24 hours, will be dried at 80 DEG C
Charcoal after dry, which is put into pulverizer, to be crushed, and then with the sieve of 100 mesh, is placed at dry and is saved, spare.
(2) it the preparation of nitrogen P Modification lotus leaf charcoal: weighs 100 mesh Lotus Leaf 5g below in the balance and is placed in beaker
In, the ammonium dibasic phosphate solution that 100mL is prepared in advance is added, beaker is put into ultrasound 4h in ultrasonic cleaning machine, is dried in 80 DEG C,
Sample after drying is ground with agate mortar, sealing is set and saved at dry.Again by the lotus leaf after nitrogen P Modification obtained above
Powder is put into be pyrolyzed in tube furnace and fire, and the leakproofness of tube furnace quartz ampoule is kept in pyrolytic process, while with 50mL/min's
Air-flow velocity is passed through N2, it is ensured that the temperature program of tube furnace: the anoxia condition in whole process quartz ampoule is heated to from room temperature
600 DEG C, 10 DEG C/min of heating rate, and 600 DEG C of conditions is kept persistently to be pyrolyzed 1 hour, then start nature and be down to room temperature, whole
N is endlessly passed through during a2And keep N2Flow velocity it is constant, after being cooled to room temperature take out.By taking-up
Charcoal, for several times until washing lotion pH value is not changed, is put into baking oven 80 DEG C of drying, obtains nitrogen P Modification lotus leaf with milli-Q water
Charcoal.
2 gained nitrogen P Modification lotus leaf charcoal of embodiment is used for the absorption of lead ion, result to be as shown in Figure 3.Nitrogen phosphorus
Modified lotus leaf charcoal is up to 315mg/g, the adsorbance of the 50mg/g of significantly larger than unmodified burnt FOLIUM NELUMBINIS to the adsorption capacity of lead.
Claims (10)
1. a kind of preparation method of nitrogen P Modification lotus leaf charcoal, which comprises the steps of:
(1) biomass raw material lotus leaf is cleaned with deionized water, lotus leaf is placed in pulverizer after drying and crushes and is sieved；
(2) ammonium dibasic phosphate solution is prepared；
(3) solid-liquid mass ratio for pressing 1:15 ~ 25, weigh Lotus Leaf obtained by step (1) be added into step (2) acquired solution it is super
It sound 3 ~ 5 hours, then dries and grinds, obtain modified Lotus Leaf；
(4) modified Lotus Leaf obtained by step (3) is put into the pyrolysis carried out in tube furnace under anoxia condition to fire, fires and completes
After be cooled to room temperature after take out；
(5) by the charcoal of taking-up with milli-Q water several times until washing lotion pH value do not change, dry again, obtain nitrogen phosphorus and change
The lotus leaf charcoal of property.
2. the preparation method of nitrogen P Modification lotus leaf charcoal according to claim 1, which is characterized in that in step (1), dry
Dry temperature is 70 ~ 110 DEG C, and drying time is 18 ~ 30 hours.
3. the preparation method of nitrogen P Modification lotus leaf charcoal according to claim 1, which is characterized in that in step (1), mistake
Screen the sieve of 100 ~ 300 mesh.
4. the preparation method of nitrogen P Modification lotus leaf charcoal according to claim 1, which is characterized in that in step (2), phosphorus
Sour two ammonium salt solution of hydrogen is added ultrapure water in volumetric flask by weighing diammonium hydrogen phosphate and is settled to scale and obtains, ammonium dibasic phosphate solution
Concentration be 0.3 ~ 1 mol/L.
5. the preparation method of nitrogen P Modification lotus leaf charcoal according to claim 1, which is characterized in that in step (4), heat
Solving temperature is 400 ~ 600 DEG C, the leakproofness of tube furnace quartz ampoule is kept in pyrolytic process, while with the air-flow of 30 ~ 60mL/min
Flow velocity is passed through N2, it is ensured that the anoxia condition in whole process quartz ampoule, the temperature program of tube furnace: 400 are heated to from room temperature ~
600 DEG C, heating rate is 5 ~ 10 DEG C/min, and 400 ~ 600 DEG C of conditions is kept persistently to be pyrolyzed 0.8 ~ 1.2 hour, is then started certainly
It so is down to room temperature, to be endlessly passed through N in the whole process2And keep N2Flow velocity it is constant.
6. the preparation method of nitrogen P Modification lotus leaf charcoal according to claim 1, which is characterized in that in step (5), dry
Dry temperature is 70 ~ 100 DEG C.
7. the nitrogen P Modification lotus leaf charcoal that preparation method as claimed in any one of claims 1 to 6 obtains is in removal water body
The application of lead ion.
8. application according to claim 7, which is characterized in that specifically includes the following steps:
The nitrogen P Modification lotus leaf charcoal that preparation method as claimed in any one of claims 1 to 6 obtains is mixed with lead waste water,
Purified solution is obtained through concussion, ultrafiltration.
9. application according to claim 8, which is characterized in that the plumbum ion concentration of the leaded ion waste water is 10 ~ 500mg/
L；The solid-to-liquid ratio of nitrogen P Modification charcoal and leaded ion waste water is the g/mL of 1:10 ~ 100.
10. application according to claim 8, which is characterized in that the revolving speed of the concussion is 100 ~ 400rpm.
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Cited By (3)
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| CN114917872A (en) * | 2022-06-27 | 2022-08-19 | 南华大学 | Aluminum nitrate modified lotus leaf biochar and preparation method and application thereof |
| CN115228499A (en) * | 2022-08-05 | 2022-10-25 | 安徽工程大学 | N-self-doped lotus leaf biochar and preparation method and application thereof |
| CN116492983A (en) * | 2023-04-25 | 2023-07-28 | 中国科学院过程工程研究所 | Rare earth element-nitrogen-phosphorus co-doped biochar and preparation method and application thereof |
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| CN115228499A (en) * | 2022-08-05 | 2022-10-25 | 安徽工程大学 | N-self-doped lotus leaf biochar and preparation method and application thereof |
| CN116492983A (en) * | 2023-04-25 | 2023-07-28 | 中国科学院过程工程研究所 | Rare earth element-nitrogen-phosphorus co-doped biochar and preparation method and application thereof |
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Application publication date: 20190903 |