CN107051386A - The carbon material of chromium ion and its preparation in a kind of energy adsorption aqueous solution - Google Patents
The carbon material of chromium ion and its preparation in a kind of energy adsorption aqueous solution Download PDFInfo
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- CN107051386A CN107051386A CN201710351254.1A CN201710351254A CN107051386A CN 107051386 A CN107051386 A CN 107051386A CN 201710351254 A CN201710351254 A CN 201710351254A CN 107051386 A CN107051386 A CN 107051386A
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- preparation
- mushroom
- carbon material
- chromium ion
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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
-
- 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
-
- 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The present invention relates to a kind of preparation method and application for the carbon material that can adsorb chromium ion.Use mushroom to prepare high performance porous carbon materials for raw material, and be applied to the absorption of chromium ion in the aqueous solution, the carbon material realizes the quick adsorption to chromium ion, and adsorption efficiency is high.It will bring good environmental benefit and economic benefit.
Description
Technical field
The invention belongs to water treatment field, and in particular to the Carbon Materials of chromium ion and its preparation in a kind of energy adsorption aqueous solution
Method.
Background technology
In recent years, in domestic relevant edible mushroom heavy metals exceeding standard report for work it is of common occurrence, focus primarily upon lead, cadmium, mercury,
Arsenic etc..Investigation of Heavy Metals report result in the edible mushroom of Sichuan province is shown：52 parts of total qualification rates of edible mushroom are only
7.69%, Cr, Cd and Hg content overproof in the edible mushroom of part, wherein Cr elements are exceeded the most serious.
Substantially there are two big reasons, one is the environmental factor based on empty gas and water, cover soil material, the second is edible mushroom itself
Enriching heavy metal ability internal factor.Some species of mushroom can produce some special protein, with these heavy metals
Ions binding, plays a part of detoxifying for oneself.But this " removing toxic substances " is only meaningful to mushroom, nonsensical to human body.From section
Learn and said in conclusion, some mushrooms have the ability of enriching heavy metal.The carbon material prepared using the mushroom for being enriched with chromium can lead to
Cross effective absorption of " blotting " realization to chromium ion.
Chromate waste water, essentially from electroplate technology, is an important sources for causing environmental pollution.For useless containing chromium
The improvement of water, the common method in this area has ferrite process, sulfite reduction method, ion-exchange resin and electrolysis.But
It is that these methods are required for purchase chemical reagent or expensive ion exchange resin, cost is higher.
The content of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides a kind of preparation side of new biological adsorption agent
Method and its application, and in particular to carbon material of energy purifying chromium-containing wastewater and preparation method thereof, the net of sewage is carried out using mushroom carbon
Change, the adsorption rate of chromium ion of the carbon material to containing in water is fast, and adsorption efficiency is high, with good environmental benefit and economy
Benefit.
The present invention is adopted the following technical scheme that, a kind of to adsorb carbon material of chromium ion and preparation method thereof including as follows
Step：
（1）Mushroom is cleaned, surface impurity, drying is removed；
（2）Mushroom after drying is crushed, in heated constant temperature 0.5-2 hours at 300-400 DEG C under argon gas protection, room is cooled to
Taken out after temperature, obtain pre- carbonized product；
（3）According to mass ratio in pre- carbonized product（1-3）:1 adds potassium hydroxide, is taken out after grinding is uniform；
（4）By step（3）Product argon gas protection under constant temperature 0.5-2 hours at 700-900 DEG C, be cooled to after room temperature and take
Go out；
（5）By step（4）Obtained product is soaked with diluted acid, is stirred 3-6 hours；
（6）By the sample suction filtration after pickling, and with deionized water rinsing to neutrality, the carbon material is obtained.
In a preferred embodiment of the present invention, described mushroom is selected from mushroom, asparagus, flat mushroom, pleurotus eryngii；It is preferred that
For flat mushroom.
In a preferred embodiment of the present invention, step（2）Pre- carburizing temperature be preferably 400 DEG C.
In a preferred embodiment of the present invention, step（3）In pre- carbonized product and potassium hydroxide mass ratio it is preferred
For 1:1.
In a preferred embodiment of the present invention, step（5）It is middle to be soaked using 10% watery hydrochloric acid.
In a preferred embodiment of the present invention, the specific surface area of described carbon material is more than 2000 m2/g。
The present invention also protects application of the above-mentioned carbon material during purifying chromium-containing wastewater.
In a preferred embodiment of the present invention, the initial concentration of described Cr VI is 600 mg/L, and pH value is 2,
Adsorption time is not more than 20min.
Compared with prior art, the present invention has the advantage that：
（1）Carbon and oxygen element content are very high in flat mushroom carbon material, and price is also relatively cheap, prepare with flourishing hole knot
The porous carbon materials of structure, its specific surface area can reach nearly 2000 m2/ g, is highly suitable as sorbent material and uses.
（2）Preparation process for carbon material carries out what identified as above technical scheme after long-term research was prepared
Carbon material shows the excellent performance expected from when carrying out adsorption cleaning to chromyl water, and in the feelings that pH is 2
Most strong to Cr VI adsorption capacity under condition, the removal rate of chromium ion, and can be in 20 min close to reaching absorption close to 100%
Balance, adsorption equilibrium speed has very high advantage.Using various concentrations adsorbent when adsorbance, sample can be obtained
Adsorption isothermal curve, it is known that sample is more suitable for non-homogeneous absorption surface, is not limited solely to mono layer adsorption, can also retouch
State as multi-molecular absorption.In the case where the initial concentration of Cr VI is 600 mg/L, adsorbance is more than 365mg/g, with good
Environmental benefit and economic benefit.
Embodiment
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, present invention specific examples below
Illustrate, but the present invention is limited to absolutely not these examples.
Material used in the present invention includes:Mushroom, purchases in the sharp wholesale markets of Beijing Tian Feng and Chinese Academy of Sciences's plant research
Institute；Potassium bichromate（Analysis is pure）, Chemical Reagent Co., Ltd., Sinopharm Group's production；Hydrochloric acid, the production of Beijing chemical reagent work；Hydroxide
Sodium, the production of Beijing Tong Guang fine chemistry industries company；Potassium hydroxide, the production of Beijing chemical reagent work.
Embodiment 1：
（1）Flat mushroom is cleaned, removes to be put into after surface impurity in baking oven and is dried under 100 DEG C of environment.
（2）Mushroom after drying is crushed, is subsequently placed in crucible and is put into tube furnace and heats.By programme-control by room temperature
300 DEG C are warming up to, the lower constant temperature of argon gas protection 1 hour is cooled to after room temperature and taken out, and now sample is pre- carbonized carbonaceous to mark.
（3）By potassium hydroxide, preparation carbon mass ratio 3:1, potassium hydroxide is added in preparation carbon, mortar grinder is put into uniform
Take out afterwards and be put into different crucibles.
（4）Crucible is put into tube furnace and heated, programme-control is by room temperature to 700 DEG C, and the lower constant temperature 1 of argon gas protection is small
When, it is cooled to after room temperature and takes out.
（5）Sample, magnetic agitation 4 hours, with the inorganic salts except generation of deactivating are soaked with 10% watery hydrochloric acid.
（6）By the sample suction filtration after pickling, and with deionized water rinsing to neutrality, obtained carbon material is labeled as MC-
700-1。
Embodiment 2：
（1）Flat mushroom is cleaned, removes to be put into after surface impurity in baking oven and is dried under 100 DEG C of environment.
（2）Mushroom after drying is crushed, is subsequently placed in crucible and is put into tube furnace and heats.By programme-control by room temperature
350 DEG C are warming up to, the lower constant temperature of argon gas protection 1 hour is cooled to after room temperature and taken out, and now sample is pre- carbonized carbonaceous to mark.
（3）By potassium hydroxide, preparation carbon mass ratio 2:1, potassium hydroxide is added in preparation carbon, mortar grinder is put into uniform
Take out afterwards and be put into different crucibles.
（4）Crucible is put into tube furnace and heated, programme-control is by room temperature to 800 DEG C, and the lower constant temperature 1 of argon gas protection is small
When, it is cooled to after room temperature and takes out.
（5）Sample, magnetic agitation 4 hours, with the inorganic salts except generation of deactivating are soaked with 10% watery hydrochloric acid.
（6）By the sample suction filtration after pickling, and with deionized water rinsing to neutrality, obtained carbon material is labeled as MC-
800-1。
Embodiment 3：
（1）Flat mushroom is cleaned, removes to be put into after surface impurity in baking oven and is dried under 100 DEG C of environment.
（2）Flat mushroom after drying is crushed, is subsequently placed in crucible and is put into tube furnace and heats.By programme-control by room temperature
400 DEG C are warming up to, the lower constant temperature of argon gas protection 1 hour is cooled to after room temperature and taken out, and now sample is pre- carbonized carbonaceous to mark.
（3）By potassium hydroxide, preparation carbon mass ratio 1:1, potassium hydroxide is added in preparation carbon, mortar grinder is put into uniform
Take out afterwards and be put into different crucibles.
（4）Crucible is put into tube furnace and heated, programme-control is by room temperature to 900 DEG C, and the lower constant temperature 1 of argon gas protection is small
When, it is cooled to after room temperature and takes out.
（5）Sample, magnetic agitation 4 hours, with the inorganic salts except generation of deactivating are soaked with 10% watery hydrochloric acid.
（6）By the sample suction filtration after pickling, and with deionized water rinsing to neutrality, obtained carbon material is labeled as MC-
900-1。
The carbon prepared is subjected to sign measure, surface topography is observed using the conventional SEM in this area, surveyed using BET method
Determine specific surface area, and to element composition and content and to chromium ion（Initial concentration is 600 mg/L）Adsorption capacity carry out
Analysis and sign.
As a result find, sample prepared by embodiment 1-3 is increased over time, and adsorbance gradually increases, when reaching about
After 20min, with the increase of adsorption time, adsorbance is held essentially constant.Illustrate the sexavalence in the carbon material absorption waste water
Chromium ion 20min is that can reach balance, it is possible to achieve Fast-Balance.Have obvious compared with other adsorbents reported in the literature
Advantage.
It is 2 to 7 from pH, Cr VI removal rate is reduced with the rise of pH value.The removal rate highest as pH=2, be
97.75%。
The sample specific surface area activated in embodiment 1-3 at different 700 DEG C, 800 DEG C and 900 DEG C of activation temperatures is respectively
1090 m2/ g, 1804 m2/ g and 1935 m2/ g, with the increase of activation temperature, specific surface area gradually increases, adsorbance also with
Increase.Also, as temperature increases, low-pressure end adsorbance gradually increases, this just illustrate the micro pore volume of the carbon material with
Activation temperature increase and increase.Meanwhile, the sample curves at 800 DEG C and 900 DEG C occur in that small time stagnant ring, illustrate material
Also containing on a small quantity mesoporous.
Although by referring to the preferred embodiments of the present invention, invention has been described, this area it is common
It will be appreciated by the skilled person that various changes can be made to it in the form and details, without departing from appended right
The spirit and scope of the present invention that claim is limited.
Claims (8)
1. a kind of can be to the preparation method of the carbon material of chromium ion high absorption property, it is characterised in that comprise the following steps：
（1）Mushroom is cleaned, surface impurity, drying is removed；
（2）Mushroom after drying is crushed, in heated constant temperature 0.5-2 hours at 300-400 DEG C under argon gas protection, room is cooled to
Taken out after temperature, obtain the product of pre- carbonization；
（3）According to mass ratio in pre- carbonized carbonaceous（1-3）:1 adds potassium hydroxide, is taken out after grinding is uniform；
（4）By step（3）Product argon gas protection under constant temperature 0.5-2 hours at 500-900 DEG C, be cooled to after room temperature and take
Go out；
（5）By step（4）Obtained product is soaked with diluted acid, stirring and washing 3-6 hours；
（6）By the sample suction filtration after pickling, and with deionized water rinsing to neutrality, the carbon material is obtained.
2. preparation method according to claim 1, it is characterised in that described mushroom be selected from mushroom, asparagus, flat mushroom,
Pleurotus eryngii；Preferably flat mushroom.
3. preparation method according to claim 1, it is characterised in that step（2）Pre- carburizing temperature be 400 DEG C.
4. preparation method according to claim 1, it is characterised in that step（3）In pre- carbonized carbonaceous and potassium hydroxide matter
Amount is than being 1:1.
5. preparation method according to claim 1, it is characterised in that step（5）It is middle to be soaked using 10% watery hydrochloric acid.
6. preparation method according to claim 1, it is characterised in that the specific surface area of described carbon material is more than 2000
m2/g。
7. the carbon material that the preparation method any one of claim 1-6 is prepared answering in chromium ion adsorption process
With.
8. application according to claim 7, it is characterised in that the initial concentration of Cr VI is in described absorption chromium ion
600 mg/L, pH value is 2, and adsorption time is not more than 20min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710351254.1A CN107051386A (en) | 2017-05-18 | 2017-05-18 | The carbon material of chromium ion and its preparation in a kind of energy adsorption aqueous solution |
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| CN201710351254.1A CN107051386A (en) | 2017-05-18 | 2017-05-18 | The carbon material of chromium ion and its preparation in a kind of energy adsorption aqueous solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107456984A (en) * | 2017-09-04 | 2017-12-12 | 山东师范大学 | Iron carbon composite and preparation method with visible ray photolysis water hydrogen performance |
| CN110707332A (en) * | 2019-09-29 | 2020-01-17 | 中国石油大学(华东) | Preparation method and application of bromine-regulated biomass-derived oxygen reduction and hydrogen evolution catalyst |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669605A (en) * | 2016-12-14 | 2017-05-17 | 北京化工大学 | Porous carbon adsorbent and preparation method and application thereof |
-
2017
- 2017-05-18 CN CN201710351254.1A patent/CN107051386A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106669605A (en) * | 2016-12-14 | 2017-05-17 | 北京化工大学 | Porous carbon adsorbent and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 臧锐: ""生物质基活性碳材料的制备及电化学性能的研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107456984A (en) * | 2017-09-04 | 2017-12-12 | 山东师范大学 | Iron carbon composite and preparation method with visible ray photolysis water hydrogen performance |
| CN110707332A (en) * | 2019-09-29 | 2020-01-17 | 中国石油大学(华东) | Preparation method and application of bromine-regulated biomass-derived oxygen reduction and hydrogen evolution catalyst |
| CN110707332B (en) * | 2019-09-29 | 2022-06-21 | 中国石油大学(华东) | Preparation method and application of bromine-regulated biomass-derived oxygen reduction and hydrogen evolution catalyst |
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Application publication date: 20170818 |