CN111892049B - Method for preparing adsorbing material by using camellia oleifera shells, adsorbing material and application thereof - Google Patents
Method for preparing adsorbing material by using camellia oleifera shells, adsorbing material and application thereof Download PDFInfo
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- CN111892049B CN111892049B CN202010668765.8A CN202010668765A CN111892049B CN 111892049 B CN111892049 B CN 111892049B CN 202010668765 A CN202010668765 A CN 202010668765A CN 111892049 B CN111892049 B CN 111892049B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
Abstract
The invention discloses a method for preparing an adsorbing material by using oil tea shells, the adsorbing material and application thereof, the adsorbing material is prepared by a method of electrolytic deliming and gradual temperature rise carbonization, and the method comprises the following steps: firstly, carrying out alkali washing; carrying out electrolytic screening on the oil tea fruit shell material subjected to alkali washing on ash components in the oil tea fruit shell; under the protection of nitrogen, carrying out gradual heating carbonization treatment; the adsorption material with high adsorption capacity is finally obtained through activation treatment by a steam activation method and a phosphoric acid soaking activation method in sequence, and then through washing with boiling water, acid washing and drying. According to the invention, by adopting the electrolytic deliming method, the pH is adjusted by adding hydrochloric acid in the electrolytic process, so that the electrolytic deliming efficiency is increased, the content of impurity elements in the shells is greatly reduced, the influence of residual impurities on the formation of micropores of the adsorption material is reduced, the total specific surface area of the adsorption material is increased, and the performance of the adsorption material is obviously improved.
Description
Technical Field
The invention relates to the technical field of preparation of adsorption materials, in particular to a method for preparing an adsorption material by using oil tea shells, the adsorption material and application thereof.
Background
The shell activated carbon is widely applied to deep purification and gas phase adsorption of drinking water, industrial water and waste water, and the application number of the prior art is '201910883381.5', and discloses a preparation method of a mixed carbon-based adsorption material for groundwater remediation, wherein the adsorption material is composed of oil tea shells with the particle size of 2-4 mm and phosphoric acid with the mass fraction of 60% as main raw materials, and the oil tea shells are 1: 2, the mixed carbon-based adsorption material is formed by the steps of carbonization, activation, boiling water washing, acid washing, drying and the like, although the method is simple to operate and easy to implement, the adsorption capacity of the adsorption material prepared by the method is poor, the adsorption material can quickly reach adsorption saturation when used for groundwater remediation, and the adsorption material needs to be replaced by workers at irregular time, so that the use cost is increased.
Therefore, the invention provides an improved method for preparing an adsorbing material by using oil tea shells, so as to solve the problem of poor adsorbing capacity of the adsorbing material.
Disclosure of Invention
The invention aims to provide a method for preparing an adsorbing material by using oil tea shells, the adsorbing material and application thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing an adsorbing material by using oil tea shells is characterized in that the adsorbing material is prepared by electrolytic deashing and gradual heating carbonization, and the specific method comprises the following steps:
mixing the oil tea shell product cracked by the plasma with a dilute alkali solution, stirring for 1-2 hours at 150-210 ℃, and carrying out alkali washing;
introducing the oil tea fruit shell material subjected to alkali washing into an electrolytic cell, wherein the solid-liquid ratio is 1: adding a proper amount of water according to the proportion of 8, uniformly mixing, adjusting the pH to 3-4 by using hydrochloric acid, standing for 1-1.5 h, electrifying to perform electrolytic screening on ash components in the oil tea fruit shell, timing and electrolyzing for 20-30 min when bubbles are generated in an electrolytic cell, and collecting oil tea fruit shell materials;
under the protection of nitrogen, transferring the dried oil tea shell material into a muffle furnace for carbonization treatment, wherein the carbonization temperature is 800-900 ℃, and the temperature is gradually increased at the temperature increasing rate of 10 ℃/min, and the carbonization time is 2.5 h;
and after carbonization, cooling to room temperature, sequentially carrying out activation treatment by a steam activation method and a phosphoric acid soaking activation method, and finally obtaining the adsorbing material with high adsorption capacity by boiling water washing, acid washing and drying.
Preferably, during electrolytic deashing, an anion exchange membrane is arranged at the anode to control the motion process of anions, and a cation exchange membrane is arranged at the cathode to control the motion process of cations.
Preferably, the electrolytic deashing treatment is carried out in an oxygen-rich environment at normal temperature and normal pressure, and the electrolytic voltage is AC 380V.
Preferably, before the carbonization treatment, the material is activated for 30-40 min by a water vapor activation device.
Preferably, the oil tea fruit shell and the dilute alkali solution are mixed according to a solid-liquid ratio of 1: 10, and the mass fraction of the dilute alkali is 10-15 percent.
The application of the adsorption material prepared from the camellia oleifera shells is obtained according to the preparation method, and the adsorption material prepared from the camellia oleifera shells is used for groundwater remediation.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the oil tea fruit shell after alkali treatment is further treated by an electrolytic deashing method, and the pH is adjusted by adding hydrochloric acid in the electrolytic process, so that the electrolytic deashing efficiency is increased, the content of impurity elements in the fruit shell is greatly reduced, the influence of residual impurities on the formation of micropores of an adsorption material is reduced, the total specific surface area of the adsorption material is increased, the adsorption capacity of the adsorption material is further increased, and the performance of the adsorption material is obviously improved; meanwhile, the temperature rise rate during carbonization is constant by adopting a step-by-step temperature rise carbonization mode, so that the phenomenon that the internal dehydration process is influenced due to the overlarge temperature difference between the inside and the outside of the shell particles is prevented, the carbonization effect is improved, and the adsorption performance of the adsorption material is obviously improved; the ash content of the adsorbing material obtained by the method for preparing the adsorbing material by using the oil tea fruit shells reaches below 1.95 percent, and the specific surface area reaches 3715m2More than g, the water-based adsorption material has good adsorption capacity, and in the process of water restoration, frequent replacement of the adsorption material by maintenance personnel is avoided, so that the water restoration cost is reduced.
Drawings
Fig. 1 is a process flow diagram of the method for preparing the adsorbing material by using the camellia oleifera shells according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
a method for preparing an adsorbing material by using oil tea shells is characterized in that the adsorbing material is prepared by electrolytic deashing and gradual heating carbonization, and the specific method comprises the following steps:
s101: mixing a plasma cracked oil tea shell product with a dilute alkali solution with the mass fraction of 10% -15% according to a solid-liquid ratio of 1: 10, mixing, stirring for 1-2 hours at 150-210 ℃, and carrying out alkali washing;
s102: introducing the oil tea fruit shell material subjected to alkali washing into an electrolytic cell, wherein the solid-liquid ratio is 1: adding a proper amount of water according to the proportion of 8, uniformly mixing, adjusting the pH value to 3-4 by using hydrochloric acid, standing for 1-1.5 h, arranging an anion exchange membrane at an anode to control the movement process of anions, arranging a cation exchange membrane at a cathode to control the movement process of cations, performing electrolytic deashing treatment in an oxygen-enriched environment at normal temperature and normal pressure, wherein the electrolytic voltage is AC380V, timing and electrolyzing for 20-30 min when bubbles are generated in an electrolytic cell, and collecting oil tea shell materials;
s103: activating the oil tea fruit shell material for 30-40 min by a water vapor activation device, and after activation, transferring the dried oil tea fruit shell material to a muffle furnace for carbonization treatment under the protection of nitrogen, wherein the carbonization temperature is 800-900 ℃, the temperature is gradually increased at the temperature increase rate of 10 ℃/min, and the carbonization time is 2.5 h;
s104: and after carbonization, cooling to room temperature, sequentially carrying out activation treatment by a steam activation method and a phosphoric acid soaking activation method, and finally obtaining the adsorbing material with high adsorption capacity by boiling water washing, acid washing and drying.
The application of the adsorbing material prepared from the camellia oleifera shells is obtained by the preparation method according to claims 1-5, and the adsorbing material prepared from the camellia oleifera shells is used for groundwater remediation.
Example (b):
mixing a plasma cracked oil tea shell product with a dilute alkali solution with the mass fraction of 10% according to a solid-liquid ratio of 1: 10, mixing, stirring for 2 hours at 150 ℃, and carrying out alkali washing;
introducing the oil tea fruit shell material subjected to alkali washing into an electrolytic cell, wherein the solid-liquid ratio is 1: adding a proper amount of water according to the proportion of 8, uniformly mixing, adjusting the pH to 3.5 by using hydrochloric acid, standing for 1.5h, arranging an anion exchange membrane at an anode to control the movement process of anions, arranging a cation exchange membrane at a cathode to control the movement process of cations, performing electrolytic deashing treatment in an oxygen-rich environment at normal temperature and normal pressure, wherein the electrolytic voltage is AC380V, timing and electrolyzing for 30min when bubbles are generated in an electrolytic cell, and collecting oil tea shell materials;
activating the oil tea fruit shell material for 40min by a water vapor activation device, and after activation, transferring the oil tea fruit shell material to a muffle furnace for carbonization treatment under the protection of nitrogen, wherein the carbonization temperature is 850 ℃, the temperature is gradually increased at the temperature increase rate of 10 ℃/min, and the carbonization time is 2.5 h;
after carbonization is finished, gradually cooling to 100 ℃ at a cooling rate of 10 ℃/min, introducing steam for 30 minutes, cooling to room temperature, and mixing the phosphoric acid solution and the carbonized oil tea fruit material according to a solid-to-liquid ratio of 1: 10, mixing and soaking for 15 hours, drying the mixed material, transferring the dried mixed material to a muffle furnace for activation under the protection of nitrogen, wherein the activation temperature is 850 ℃, the temperature is gradually increased at the temperature increase rate of 50 ℃/min, the activation time is 30min, washing the activated material for 15 minutes by boiling water, washing the washed material by dilute hydrochloric acid, washing the washed material by distilled water for multiple times, and finally drying the washed material at 120 ℃ to obtain the adsorbing material with high adsorption capacity;
taking 2000g of the adsorbing material, detecting the ash content of the adsorbing material and determining the specific surface area of the adsorbing material, and through inspection, the ash content of the adsorbing material obtained by the method reaches below 1.95 percent, and the specific surface area reaches 3715m2The adsorption capacity is good, frequent replacement of the adsorption material by maintenance personnel is avoided in the water restoration process, and the water restoration cost is reduced.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for preparing an adsorbing material by using oil tea shells is characterized in that the adsorbing material is prepared by a method of electrolytic deashing and gradual temperature rise carbonization, and the specific method comprises the following steps:
mixing the oil tea shell product cracked by the plasma with a dilute alkali solution, stirring for 1-2 hours at 150-210 ℃, and carrying out alkali washing;
introducing the oil tea fruit shell material subjected to alkali washing into an electrolytic cell, wherein the solid-liquid ratio is 1: adding a proper amount of water according to the proportion of 8, uniformly mixing, adjusting the pH to 3-4 by using hydrochloric acid, standing for 1-1.5 h, electrifying to perform electrolytic screening on ash components in the oil tea fruit shell, timing and electrolyzing for 20-30 min when bubbles are generated in an electrolytic cell, and collecting oil tea fruit shell materials;
under the protection of nitrogen, transferring the dried oil tea shell material into a muffle furnace for carbonization treatment, wherein the carbonization temperature is 800-900 ℃, and the temperature is gradually increased at the temperature increasing rate of 10 ℃/min, and the carbonization time is 2.5 h;
and after carbonization, cooling to room temperature, sequentially carrying out activation treatment by a steam activation method and a phosphoric acid soaking activation method, and finally obtaining the adsorbing material with high adsorption capacity by boiling water washing, acid washing and drying.
2. The method for preparing the adsorbing material by using the camellia oleifera shells according to claim 1, wherein the method comprises the following steps: during electrolysis and deashing, an anion exchange membrane is arranged at the anode to control the motion process of anions, and a cation exchange membrane is arranged at the cathode to control the motion process of cations.
3. The method for preparing the adsorbing material by using the camellia oleifera shells according to claim 1, wherein the method comprises the following steps: the electrolytic deashing treatment is carried out in an oxygen-rich environment at normal temperature and normal pressure, and the electrolytic voltage is AC 380V.
4. The method for preparing the adsorbing material by using the camellia oleifera shells according to claim 1, wherein the method comprises the following steps: before carbonization, the material is activated for 30-40 min by a steam activation device.
5. The method for preparing the adsorbing material by using the camellia oleifera shells according to claim 1, wherein the method comprises the following steps: the oil tea fruit shell and the dilute alkali solution are mixed according to the solid-liquid ratio of 1: 10, and mixing the diluted alkali with the mass fraction of 10-15%.
6. The application of the adsorption material prepared from the camellia oleifera shells is characterized in that: the adsorbing material is obtained by the preparation method according to any one of claims 1-5, and the adsorbing material prepared from the camellia oleifera shells is used for groundwater remediation.
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CN110078070A (en) * | 2019-04-11 | 2019-08-02 | 西安石油大学 | A kind of preparation method of the oily sludge base absorption carbon material for oily waste water treatment |
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