CN110354802A - A method of heavy-metal adsorption material is prepared by raw material of stub - Google Patents
A method of heavy-metal adsorption material is prepared by raw material of stub Download PDFInfo
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- CN110354802A CN110354802A CN201910569158.3A CN201910569158A CN110354802A CN 110354802 A CN110354802 A CN 110354802A CN 201910569158 A CN201910569158 A CN 201910569158A CN 110354802 A CN110354802 A CN 110354802A
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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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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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
- B01J2220/4812—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
- B01J2220/4831—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton having been subjected to further processing, e.g. paper, cellulose pulp
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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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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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
Abstract
The present invention provides a kind of methods for preparing heavy-metal adsorption material as raw material using stub, include the following steps: that stub 1) is removed wrapping paper, crushing obtains fluffy powder, it takes fluffy powder to be added to the water to react at 200-300 DEG C, reaction terminates to be cooled to room temperature, washing centrifugation product, is dried to obtain solid material;2) solid material obtained by step 1) is uniformly mixed with potassium hydroxide, under the protection of inert gas, is reacted at 400-600 DEG C in high temperature furnace;Reaction terminates to be cooled to room temperature, and collects solid material;3) it by step 2) obtained solid material, is adjusted to neutrality with acid solution, and dry, obtains adsorbent material.Stub is carried out hydro-thermal reaction by the present invention, using subsequent processings such as activation, cleaning-dryings, finally obtains the carbon material for adsorbing lead ion in water.The present invention has many advantages, such as that raw material is easy to get, prepares that simple, low in cost, environmentally protective, adsorption effect is good.
Description
Technical field
The invention belongs to technical field of adsorption material preparation, and in particular to a kind of to prepare heavy metal suction by raw material of stub
The method of enclosure material.
Background technique
Lead is one of the metal that the mankind have found earliest, it is very universal in nature.The toxicity of lead is a kind of potential
Toxicity can all generate serious disorder to the nervous centralis of human body, hemopoietic system, liver system, renal system etc., cause serious
Disease.The acute toxicity of lead is very rare and related with exposure caused by mankind's occupation, and chronic toxicity is very universal, occurs
When Pb-B is about 40-60 μ g/dL.The unique property that lead possesses, such as: flexibility, high ductibility, low melting point and
It is widely applied in a variety of industry such as automobile, paint, ceramics, plastics in corrosion resistance.This also results in the lead of free state in life
State system and increasing in inert environments.The not biodegradable property of lead make its can long-term existence in ambient water
In body, environment and human body are generated and greatly threatened.Therefore, the lead ion removed in water body is very necessary.
Currently, the method for removal Lead in Aqueous Solution has very much, mainly there are chemical precipitation method, ion-exchange, film filtering
The methods of method, electrochemistry, absorption method, reverse osmosis, bioanalysis.Absorption method therein is because adsorbent is cheap and easy to get, low energy consumption, does not produce
It is raw secondary pollution, not high to equipment requirement, it is one of most efficient method, and absorbent charcoal material is common adsorbent.
Stub is a kind of important solid waste, it is estimated that the every annual meeting in the whole world generates about 5.8 trillion stubs, gross weight
Amount is more than 800,000 tons.The random discarding of stub can not only generate a large amount of rubbish, and the harmful substances such as nicotine contained therein can
It can be discharged into environment, harm is generated to wild animal and human health.The material of stub is mainly acetate fiber, using it as
Carbon source can prepare absorption of the absorbent charcoal material for lead ion, be a kind of approach to turn waste into wealth.
Summary of the invention
The purpose of the invention is to overcome defect of the existing technology, provide a kind of using stub as raw material preparation weight
The method of metal-adsorbing material obtains the carbon material for being used to adsorb lead ion in water after efficiently using stub.
To achieve the goals above, in the embodiment on basis, the present invention provides one kind using stub as raw material system
The method of standby heavy-metal adsorption material, includes the following steps:
1) hydrothermal carbonization: stub is removed into wrapping paper, crushing obtains fluffy powder, fluffy powder is taken to be added to the water in 200-
It is reacted at 300 DEG C, reaction terminates to be cooled to room temperature, and washing centrifugation product is dried to obtain solid material;
2) it activates: solid material obtained by step 1) is uniformly mixed with potassium hydroxide, under the protection of inert gas, in
It is reacted at 400-600 DEG C in high temperature furnace;Reaction terminates to be cooled to room temperature, and collects solid material;
3) it is cleaned and dried: step 2) obtained solid material being adjusted to neutrality with acid solution, is cleaned with pure water and is done afterwards three times
It is dry, obtain adsorbent material.
In a preferred embodiment, fluffy powder described in step 1) and water quality ratio are 1:8-12.
In a preferred embodiment, the temperature program of reaction described in step 1) is, with the rate of 3-5 DEG C/min
It is warming up to 200-300 DEG C, and keeps being cooled to room temperature with the rate of 3-5 DEG C/min after 1.5-2.5h.
In a preferred embodiment, drying temperature described in step 1) is 110-115 DEG C.
In a preferred embodiment, fluffy powder described in step 1) and water quality ratio are 1:10;
Temperature program is reacted described in step 1) are as follows: be warming up to 250 with the rate of 5 DEG C/min, and after keeping 2h under 250
Room temperature is cooled to the rate of 5 DEG C/min;
Drying temperature described in step 1) is 112 DEG C.
In a preferred embodiment, the quality in step 2) through solid material obtained by step 1) and potassium hydroxide
Than for 1:3-5.
In a preferred embodiment, high temperature furnace temperature program described in step 2) is with the rate of 3-5 DEG C/min
It is warming up to 450-550 DEG C, is cooled down after keeping 1-2h.
In a preferred embodiment, the matter through step 1) obtained solid material and potassium hydroxide in step 2)
Amount is than being 1:4;
High temperature furnace temperature program described in step 2) is that 500 DEG C are warming up to the rate of 3 DEG C/min, is cooled down after keeping 1h.
In a preferred embodiment, acid solution described in step 3) is the HCl solution of 1-3mol/L.
In a preferred embodiment, drying temperature described in step 3) is 110-115 DEG C.
In a preferred embodiment, acid solution described in step 3) is the HCl solution of 2mol/L;Institute in step 3)
Stating drying temperature is 112 DEG C.
Through the above technical solutions, stub is carried out hydro-thermal reaction by the method for the present invention, after activation, cleaning-drying etc.
Continuous processing, finally obtains the carbon material for adsorbing lead ion in water.The present invention provides outlet for the recovery processing of stub, with
Stub is carbon source, and abundance is environmentally protective.Meanwhile the carbon material obtained by the method for the invention, rich in oxygen-containing group and height
Specific surface area has good effect to the processing of Lead in Aqueous Solution, can make tribute for the improvement of heavy metal in water body environment
It offers.
Detailed description of the invention
Fig. 1 is 1 stub powder electron-microscope scanning figure of the embodiment of the present invention.
Fig. 2 is the material electron-microscope scanning figure that 1 stub powder of the embodiment of the present invention obtains after 250 DEG C of hydro-thermals.
Fig. 3 is that 2 stub powder hydrothermal carbonization of the embodiment of the present invention activates obtained absorbent charcoal material through 500 DEG C again later
Electron-microscope scanning figure.
Fig. 4 is that 2 stub powder hydrothermal carbonization of the embodiment of the present invention activates obtained absorbent charcoal material through 500 DEG C again later
Infrared spectrogram.
Specific embodiment
In order to better understand the above technical scheme, being done below by specific embodiment to technical scheme detailed
Explanation, it should be understood that the specific features in the embodiment of the present application and embodiment be to technical scheme specifically
It is bright, rather than the restriction to technical scheme, in the absence of conflict, the skill in the embodiment of the present application and embodiment
Art feature can be combined with each other.It should be understood that term "and/or" used herein above includes listed by one of them or more
Any and all combinations of associated item out.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The main thought of the embodiment of the present invention is: a method of heavy-metal adsorption material being prepared by raw material of stub,
Include the following steps:
1) hydrothermal carbonization: stub is removed into wrapping paper, crushing obtains fluffy powder, fluffy powder is taken to be added to the water in 200-
It is reacted at 300 DEG C, reaction terminates to be cooled to room temperature, and washing centrifugation product is dried to obtain solid material;
2) it activates: solid material obtained by step 1) is uniformly mixed with potassium hydroxide, under the protection of inert gas, in
It is reacted at 400-600 DEG C in high temperature furnace;Reaction terminates to be cooled to room temperature, and collects solid material;
3) it is cleaned and dried: step 2) obtained solid material being adjusted to neutrality with acid solution, is cleaned with pure water and is done afterwards three times
It is dry, obtain adsorbent material.
Above-mentioned steps 3) in adjust pH value using acid solution be and to make the oxygen-containing group of material to remove extra alkali
Group keeps activity, goes on smoothly that (adsorption experiment need to carry out under the conditions of pH slant acidity to prevent convenient for the adsorption experiment of next step
The hydrolysis of metal ion).
Specifically, fluffy powder described in step 1) and water quality ratio are 1:8-12, guarantee being suitble to for carbonizing degree.
Specifically, the temperature program of reaction described in step 1) is to be warming up to 200-300 DEG C with the rate of 3-5 DEG C/min,
And it keeps being cooled to room temperature with the rate of 3-5 DEG C/min after 1.5-2.5h.
Specifically, drying temperature described in step 1) is 110-115 DEG C.The temperature can guarantee going completely for vapor
It removes, and avoids the mass deficit of adsorbent material as far as possible.
Specifically, the mass ratio through solid material obtained by step 1) and potassium hydroxide in step 2) is 1:3-5.General ratio
Example is 2 to 5, and potassium hydroxide is excessive in order to guarantee that material sufficiently activates.
Specifically, high temperature furnace temperature program described in step 2) is to be warming up to 450- with the rate of 3-5 DEG C/min
550 DEG C, cool down after keeping 1-2h.The carbon material adsorption effect generated in the temperature range is best.
Specifically, acid solution described in step 3) is the HCl solution of 1-3mol/L.Hydrogen chloride can become in the drying process
At gaseous volatilization, impurity will not be introduced.The a large amount of alkali used when the use of the concentration being to neutralize activation, so that material is quick
Reach neutral.
Specifically, drying temperature described in step 3) is 110-115 DEG C.The temperature can guarantee going completely for vapor
The mass deficit removed, and avoided as far as possible.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the embodiment of the present invention
It is commercially available or can be prepared by existing method by market.
Embodiment 1
Original stub is removed into wrapping paper, crushing obtains fluffy powder, and electron microscope photo scanning is shown in Fig. 1.Take 5g
Fluffy powder, which is added 50ml ultrapure water and is placed in stainless steel cauldron, to react, and sets reaction kettle temperature program to 5 DEG C/min
Rate be warming up to 250 DEG C, and room temperature is cooled to the rate of 5 DEG C/min after keeping 2h at 250 DEG C.With milli-Q water from
Heart product, and be dried overnight at 112 DEG C, electron microscope photo scanning is shown in Fig. 2.Take dry acquired material 0.5g and 2g hydroxide
Potassium is uniformly mixed, and is placed on aluminium boat, under the protection of nitrogen, is reacted in horizontal chamber furnace (oven), and horizontal chamber furnace (oven) temperature program is with 3 DEG C/min
Rate be warming up to 400 DEG C, cool down after keeping 1h.It is cooled to room temperature, collects product, adjust product with the HCl solution of 2mol/L
To neutrality, finally it is dried overnight at 112 DEG C.Obtain the porous carbon materials of black.PH=5 is prepared, concentration is followed successively by 100,
200,300,325,350,375,400mg/L lead ion standard solution takes the above-mentioned solution of 5ml that 3mg porous carbon is added respectively
Material is placed in shaking table concussion 3h in room temperature.Rising for the lead ion solution of absorption front and back is measured using inductivity coupled plasma mass spectrometry
Beginning concentration and equilibrium concentration are calculated by the adsorption capacity of porous carbon materials according to formula, as shown in table 1.
Embodiment 2
Original stub is removed into wrapping paper, crushing obtains fluffy powder.Take 5g fluffy powder that 50ml is added ultrapure
Water, which is placed in stainless steel cauldron, to react, and sets being warming up to 250 DEG C with the rate of 5 DEG C/min for reaction kettle temperature program, and
Room temperature is cooled to the rate of 5 DEG C/min after holding 2h at 250 DEG C.Product, and the mistake at 112 DEG C are centrifuged with milli-Q water
Night is dry.It takes dry acquired material 0.5g to be uniformly mixed with 2g potassium hydroxide, is placed on aluminium boat, under the protection of nitrogen, in
It is reacted in horizontal chamber furnace (oven), horizontal chamber furnace (oven) temperature program is that 500 DEG C are warming up to the rate of 3 DEG C/min, is cooled down after keeping 1h.It is down to room temperature
Afterwards, product is collected, product is adjusted to neutrality with 2mol/L HCl, is finally dried overnight at 112 DEG C.Obtain the porous of black
Carbon material, electron microscope photo scanning are shown in Fig. 3, and infrared spectrogram is shown in Fig. 4.PH=5 is prepared, concentration is followed successively by 100,200,300,
325,350,375,400mg/L lead ion standard solution takes the above-mentioned solution of 5ml that 3mg porous carbon materials are added, in room temperature respectively
It is placed in shaking table concussion 3h.The initial concentration peace of the lead ion solution of absorption front and back is measured using inductivity coupled plasma mass spectrometry
Weigh concentration, the adsorption capacity of porous carbon materials is calculated by according to formula, as shown in table 1.
Embodiment 3
Original stub is removed into wrapping paper, crushing obtains fluffy powder.Take 5g fluffy powder that 50ml is added ultrapure
Water, which is placed in stainless steel cauldron, to react, and sets being warming up to 250 DEG C with the rate of 5 DEG C/min for reaction kettle temperature program, and
Room temperature is cooled to the rate of 5 DEG C/min after holding 2h at 250 DEG C.Product, and the mistake at 112 DEG C are centrifuged with milli-Q water
Night is dry.It takes dry acquired material 0.5g to be uniformly mixed with 2g potassium hydroxide, is placed on aluminium boat, under the protection of nitrogen, in
It is reacted in horizontal chamber furnace (oven), horizontal chamber furnace (oven) temperature program is that 600 DEG C are warming up to the rate of 3 DEG C/min, is cooled down after keeping 1h.It is down to room temperature
Afterwards, product is collected, product is adjusted to neutrality with 2mol/L HCl, is finally dried overnight at 112 DEG C.Obtain the porous of black
Carbon material.PH=5 is prepared, concentration is followed successively by 100,200,300,325,350,375,400mg/L lead ion standard solution, point
It does not take the above-mentioned solution of 5ml that 3mg porous carbon materials are added, is placed in shaking table concussion 3h in room temperature.Using inductively coupled plasma constitution
The initial concentration and equilibrium concentration of the lead ion solution of spectrum measurement absorption front and back, the suction of porous carbon materials is calculated by according to formula
Attached capacity, as shown in table 1.
Embodiment 4
Used stub is removed into wrapping paper, crushing obtains fluffy powder.Take 5g fluffy powder that 50ml ultrapure water is added
It is placed in stainless steel cauldron and reacts, set being warming up to 250 DEG C with the rate of 5 DEG C/min for reaction kettle temperature program, and
Room temperature is cooled to the rate of 5 DEG C/min after holding 2h at 250 DEG C.It is centrifuged product with milli-Q water, and at 112 DEG C overnight
It is dry.It takes dry acquired material 0.5g to be uniformly mixed with 2g potassium hydroxide, is placed on aluminium boat, under the protection of nitrogen, in sleeping
It is reacted in formula furnace, horizontal chamber furnace (oven) temperature program is that 500 DEG C are warming up to the rate of 3 DEG C/min, is cooled down after keeping 1h.It is down to room temperature
Afterwards, product is collected, product is adjusted to neutrality with 2mol/L HCl, is finally dried overnight at 112 DEG C.Obtain the porous of black
Carbon material.PH=5 is prepared, concentration is followed successively by 100,200,300,325,350,375,400mg/L lead ion standard solution, point
It does not take the above-mentioned solution of 5ml that 3mg porous carbon materials are added, is placed in shaking table concussion 3h in room temperature.Using inductively coupled plasma constitution
The initial concentration and equilibrium concentration of the lead ion solution of spectrum measurement absorption front and back, the suction of porous carbon materials is calculated by according to formula
Attached capacity, as shown in table 1.
Table 1
Embodiment 5
Original stub is removed into wrapping paper, crushing obtains fluffy powder, and electron microscope photo scanning is shown in Fig. 1.Take 5g
Fluffy powder, which is added 40ml ultrapure water and is placed in stainless steel cauldron, to react, and sets reaction kettle temperature program to 3 DEG C/min
Rate be warming up to 200 DEG C, and room temperature is cooled to the rate of 3 DEG C/min after keeping 2.5h at 200 DEG C.Use milli-Q water
It is centrifuged product, and is dried overnight at 110 DEG C, electron microscope photo scanning is shown in Fig. 2.Take dry acquired material 0.5g and 1.5g hydrogen
Potassium oxide is uniformly mixed, and is placed on aluminium boat, under the protection of nitrogen, is reacted in horizontal chamber furnace (oven), and horizontal chamber furnace (oven) temperature program is with 5
DEG C/rate of min is warming up to 500 DEG C, cool down after keeping 1.5h.It is cooled to room temperature, collects product, it is molten with the HCl of 1.5mol/L
Liquid adjusts product to neutrality, is finally dried overnight at 110 DEG C.Obtain the porous carbon materials of black.
Embodiment 6
Original stub is removed into wrapping paper, crushing obtains fluffy powder.Take 5g fluffy powder that 60ml is added ultrapure
Water, which is placed in stainless steel cauldron, to react, and sets being warming up to 300 DEG C with the rate of 5 DEG C/min for reaction kettle temperature program, and
Room temperature is cooled to the rate of 5 DEG C/min after holding 1.5h at 300 DEG C.It is centrifuged product with milli-Q water, and at 115 DEG C
It is dried overnight.It takes dry acquired material 0.5g to be uniformly mixed with 2.5g potassium hydroxide, is placed on aluminium boat, in the protection of nitrogen
Under, it is reacted in horizontal chamber furnace (oven), horizontal chamber furnace (oven) temperature program is that 550 DEG C are warming up to the rate of 3 DEG C/min, is cooled down after keeping 1.5h.
It is cooled to room temperature, collects product, adjust product to neutrality with 3mol/L HCl, be finally dried overnight at 115 DEG C.It obtains black
The porous carbon materials of color.
Referring to embodiment 1-3, the oxygen content for the material that the embodiment of the present invention obtains is increased with activation temperature and is reduced, and compares table
Area is increased with temperature with activation and is increased, and 500 DEG C of material has good table in oxygen content, specific surface area and aperture
It is existing, and adsorption capacity highest, therefore 500 DEG C are optimal activation temperature.Referring to embodiment 2 and 4, used stub ratio does not make
Although used specific surface area and aperture decrease, oxygen content increase is more, and it is higher to be eventually exhibited as adsorption capacity.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of method for preparing heavy-metal adsorption material as raw material using stub, characterized by the following steps:
1) stub being removed into wrapping paper, crushing obtains fluffy powder, takes fluffy powder to be added to the water and react at 200-300 DEG C,
Reaction terminates to be cooled to room temperature, and washing centrifugation product is dried to obtain solid material;
2) solid material obtained by step 1) is uniformly mixed with potassium hydroxide, under the protection of inert gas, in high temperature furnace
It is reacted at 400-600 DEG C;Reaction terminates to be cooled to room temperature, and collects solid material;
3) it by step 2) obtained solid material, is adjusted to neutrality, is washed and dried with acid solution, obtain adsorbent material.
2. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
1) fluffy powder described in and water quality ratio are 1:8-12.
3. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
1) temperature program of reaction described in be warming up to 200-300 DEG C with the rate of 3-5 DEG C/min, and keep after 1.5-2.5h with
The rate of 3-5 DEG C/min is cooled to room temperature.
4. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
1) drying temperature described in is 110-115 DEG C.
5. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
1) fluffy powder described in and water quality ratio are 1:10;
Temperature program is reacted described in step 1) are as follows: be warming up to 250 with the rate of 5 DEG C/min, and with 5 after keeping 2h under 250
DEG C/rate of min is cooled to room temperature;
Drying temperature described in step 1) is 112 DEG C.
6. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
2) mass ratio through solid material obtained by step 1) and potassium hydroxide in is 1:3-5.
7. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
2) high temperature furnace temperature program described in is that 450-550 DEG C is warming up to the rate of 3-5 DEG C/min, is cooled down after keeping 1-2h.
8. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
2) mass ratio through the obtained solid material of step 1) and potassium hydroxide in is 1:4;
High temperature furnace temperature program described in step 2) is that 500 DEG C are warming up to the rate of 3 DEG C/min, is cooled down after keeping 1h.
9. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
3) drying temperature described in is 110-115 DEG C.
10. the method for preparing heavy-metal adsorption material as raw material using stub according to claim 1, it is characterised in that: step
It is rapid 3) described in acid solution be 2mol/L HCl solution;
Drying temperature described in step 3) is 112 DEG C.
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CN111530465A (en) * | 2020-05-26 | 2020-08-14 | 湘潭大学 | Preparation method of supported cigarette end porous carbon material catalyst and application of supported cigarette end porous carbon material catalyst in nitrocyclohexane hydrogenation reaction |
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