CN113318709A - Oil stain adsorbent and preparation method thereof - Google Patents
Oil stain adsorbent and preparation method thereof Download PDFInfo
- Publication number
- CN113318709A CN113318709A CN202110624339.9A CN202110624339A CN113318709A CN 113318709 A CN113318709 A CN 113318709A CN 202110624339 A CN202110624339 A CN 202110624339A CN 113318709 A CN113318709 A CN 113318709A
- Authority
- CN
- China
- Prior art keywords
- oil stain
- adsorbent
- preparing
- modified
- activated carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- 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
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an oil stain adsorbent and a preparation method thereof, and relates to the technical field of adsorbents. When the oil stain adsorbent is prepared, modified activated carbon is prepared, a carbonaceous material and hydrotalcite are mixed, pressed and formed, and then preliminarily activated under a sealed condition, when the pressure of a sealed space is not changed, the mixture is immediately transferred into a potassium carbonate solution, slowly cooled and ventilated in a pressure-variable closed container, and secondary carbon activation is carried out under the atmosphere of circulating airflow; the specific surface area of the product is improved while the process steps are simplified, the residue of potassium hydroxide is not generated, the activation is more sufficient, and modified activated carbon with higher specific surface area and porosity is formed; soaking modified activated carbon in the modified chitosan solution, preserving heat, drying after a period of time, and blasting air to prepare an oil stain adsorbent; the oil stain adsorbent prepared by the invention not only has improved lipophilicity, but also has stronger adsorption capacity.
Description
Technical Field
The invention relates to the technical field of adsorbents, and particularly relates to an oil stain adsorbent and a preparation method thereof.
Background
When oil and water separation is carried out, when the oil content in the water body is large, most of oil stains in the water body can be removed by adopting a mechanical separation technology, but a small amount of oil stains still remain in the water body. These oily stains can no longer be removed by physical means such as machinery, and are dispersed in water in the form of emulsified oil in the process of removal by physical means such as machinery, so that the residual oily stains are difficult to remove.
The existing adsorbent is only made an article on the adsorption capacity, the oil stain adsorption effect brought by lipophilicity when the emulsified oil is adsorbed is not considered, and if the adsorbent with lipophilicity can be prepared, the adsorbent has a great development prospect. Therefore, the invention researches and prepares the oil stain absorbent which has lipophilicity and strong adsorption capacity.
Disclosure of Invention
The invention aims to provide an oil stain adsorbent and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the above technical problem, a first aspect of the present invention provides the following technical solutions: the preparation method of the oil stain adsorbent is characterized in that the process flow for preparing the oil stain adsorbent is as follows:
preparing an adsorbent blank, pressing and forming, primarily activating, secondarily activating, preparing modified chitosan, and preparing an oil stain adsorbent.
Preferably, the method comprises the following specific steps:
(1) uniformly mixing a carbonaceous material and hydrotalcite to prepare a mixed material, placing the mixed material into a ball mill for ball milling, wherein the ball milling time is 1.5-3 h, and sieving the mixed material with a 100-mesh sieve;
(2) adding coal tar into the sieved mixed material, uniformly stirring, and then pressing and forming to obtain an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment, and detecting the pressure of the closed environment at the same time until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent substrate into a potassium carbonate solution with the mass fraction of 10-30%, carrying out secondary activation in a pressure-variable closed container, cooling, introducing inert gas into the potassium carbonate solution, circulating until the solution is evaporated to dryness, recording the time for completely evaporating the solution to dryness, and obtaining modified activated carbon, wherein the total circulating time is three times of the time for completely evaporating to dryness;
(5) mixing chitosan, glacial acetic acid and deionized water according to a mass ratio of 5: 2: 18, heating in water bath to 80 ℃, uniformly stirring at constant temperature, adding stearic acid with the mass of 0.6 time that of the chitosan, and stirring until the stearic acid is dissolved to prepare a modified chitosan solution;
(6) and soaking the modified activated carbon in the modified chitosan solution, heating to 150-200 ℃, stirring while preserving heat for 20-30 min, drying to constant weight, and blowing to obtain a finished product.
Preferably, in the step (1): the hydrotalcite is calcium aluminum hydrotalcite; the mass ratio of the carbonaceous material to the hydrotalcite is 8: 1-10: 1.
preferably, in the step (2): the mass ratio of the coal tar to the mixed material is 1: 8-1: 10.
preferably, in the step (3): the primary activation temperature is 850-1100 ℃.
Preferably, in the step (4): the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: 50-1: 80; cooling to 700-900 ℃, wherein the cooling rate is 50 ℃/h; the inert gas is introduced at a rate of 3-5L/h.
Preferably, in the step (6): the mass ratio of the modified activated carbon to the modified chitosan solution is 1: 5-1: 8; the stirring speed is 200-400 rpm; the air speed is 0.05-0.08 m/s during air blowing, and the time is 2-3 min.
In a second aspect of the invention, a preparation method of an oil stain adsorbent is characterized in that the oil stain adsorbent prepared by the preparation method of the oil stain adsorbent comprises the following raw materials in parts by weight: 1-2 parts of modified activated carbon and 2-4 parts of modified chitosan.
Preferably, the modified activated carbon is prepared by mixing a carbonaceous material and hydrotalcite and performing primary activation and secondary activation; the modified chitosan is prepared by grafting stearic acid on chitosan.
Compared with the prior art, the invention has the following beneficial effects:
when the oil stain absorbent is prepared, modified activated carbon is prepared; mixing, pressing and forming a carbonaceous material and hydrotalcite, then carrying out primary activation under a sealed condition, immediately transferring the mixture into a potassium carbonate solution when the pressure of a sealed space is not changed, slowly cooling and ventilating in a pressure-variable closed container, and carrying out secondary carbon activation under the atmosphere of circulating airflow; the calcium-aluminum hydrotalcite is thermally decomposed to form nano calcium oxide and aluminum oxide with good dispersibility during primary activation at high temperature, the calcium oxide and the aluminum oxide are dispersed in macropores of the carbonaceous material, the specific surface area of the product is improved, carbon dioxide released by carbonate decomposition is directly subjected to primary activation on the carbonaceous material, the carbon dioxide overflows from the inside of the carbonaceous material while the process steps are simplified, the primary activation is more sufficient, carbon compounds remained in the activated carbon are decomposed, impurities are removed, blocked gaps are reopened, and the adsorption performance of the product is enhanced; transferring the mixture into a potassium carbonate solution, slowly heating, then infiltrating the potassium carbonate solution into the material, decomposing to release carbon dioxide to generate potassium oxide, ejecting calcium oxide and aluminum oxide at macropores by the carbon dioxide to reduce the pore diameter of the macropores, forming potassium hydroxide solid particles in the potassium oxide in a water vapor atmosphere, mixing the carbon dioxide and the water vapor with potassium hydroxide steam and circulating air flow to perform secondary activation, and performing carbon activation by the method to form modified activated carbon with higher specific surface area and porosity.
Soaking modified activated carbon in the modified chitosan solution, preserving heat, drying after a period of time, and blasting air to prepare an oil stain adsorbent; the modified chitosan is prepared by grafting stearic acid on chitosan, and lipophilicity of the chitosan is improved due to introduction of long-chain alkyl; when the activated carbon is soaked in the modified chitosan solution, the modified chitosan fills pores, and the dried modified chitosan is deposited on the surface and in the pores of the activated carbon, so that the specific surface area of the activated carbon is increased, and the capacity of absorbing oil stains is enhanced; after slight air blasting is carried out, modified chitosan deposited in gaps of calcium oxide and aluminum oxide at the large holes is removed, so that the adsorption capacity of the product is maximized; in the heat preservation process, stearic acid grafted on the modified chitosan is coated on the surface of calcium oxide in a chemical adsorption mode, and the calcium oxide is modified into a hydrophobic surface, so that the product is more suitable for adsorbing oil stains.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to describe the method for testing each index of the oil stain absorbent prepared in the following examples as follows:
adsorption performance: the prepared oil stain adsorbents of examples 1 and 2 and comparative examples 1, 2 and 3 were used for adsorbing oil-containing sewage containing 5%, and oil removal rate detection was performed.
Lipophilicity: the oil stain adsorbents prepared in the preparation examples 1 and 2 and the comparative example 3 are uniformly dispersed in deionized water with the same volume, and are fished out after being uniformly dispersed, and the quality is measured again, wherein the smaller the quality is, the poorer the hydrophilicity is, and the better the lipophilicity is.
Example 1
An oil stain absorbent mainly comprises the following components in parts by weight:
1 part of modified activated carbon and 2 parts of modified chitosan;
the preparation method of the oil stain adsorbent comprises the following steps:
(1) mixing a carbonaceous material and calcium-aluminum hydrotalcite according to a mass ratio of 8: 1, uniformly mixing to prepare a mixed material, placing the mixed material into a ball mill for ball milling, wherein the ball milling time is 1.5h, and sieving by a 100-mesh sieve;
(2) adding coal tar with the mass of 0.125 times of that of the sieved mixed material into the mixed material, uniformly stirring, and then pressing and forming to obtain an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment at 850 ℃, and simultaneously detecting the pressure of the closed environment until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent matrix into a potassium carbonate solution with the mass fraction of 10% to perform secondary activation in a pressure-variable closed container, wherein the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: 50, cooling to 700 ℃, wherein the cooling rate is 50 ℃/h, introducing inert gas into the potassium carbonate solution, circulating until the solution is evaporated to dryness, introducing the inert gas at a rate of 3L/h, recording the time for completely evaporating the solution to dryness, and the total circulating time is three times of the time for completely evaporating to dryness to prepare modified activated carbon;
(5) mixing chitosan, glacial acetic acid and deionized water according to a mass ratio of 5: 2: 18, heating in water bath to 80 ℃, uniformly stirring at constant temperature, adding stearic acid with the mass of 0.6 time that of the chitosan, and stirring until the stearic acid is dissolved to prepare a modified chitosan solution;
(6) soaking modified activated carbon in a modified chitosan solution, wherein the mass ratio of the modified activated carbon to the modified chitosan solution is 1: and 5, heating to 150 ℃, keeping the temperature for 20min while stirring, drying to constant weight at the stirring speed of 200rpm, and blowing at the air speed of 0.05m/s for 2min to obtain the finished product.
Example 2
An oil stain absorbent mainly comprises the following components in parts by weight:
1 part of modified activated carbon and 2 parts of modified chitosan;
the preparation method of the oil stain adsorbent comprises the following steps:
(1) mixing a carbonaceous material and calcium-aluminum hydrotalcite according to a mass ratio of 10: 1, uniformly mixing to prepare a mixed material, placing the mixed material into a ball mill for ball milling, wherein the ball milling time is 3 hours, and sieving the mixed material by a 100-mesh sieve;
(2) adding coal tar with the mass of 0.1 time of that of the sieved mixture into the sieved mixture, uniformly stirring, and then pressing and forming to obtain an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment at 1100 ℃, and simultaneously detecting the pressure of the closed environment until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent matrix into a potassium carbonate solution with the mass fraction of 30% to perform secondary activation in a pressure-variable closed container, wherein the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: 80, cooling to 900 ℃, wherein the cooling rate is 50 ℃/h, introducing inert gas into the potassium carbonate solution, circulating until the solution is evaporated to dryness, introducing the inert gas at a rate of 5L/h, recording the time for completely evaporating the solution to dryness, and obtaining the modified activated carbon, wherein the total circulating time is three times of the time for completely evaporating to dryness;
(5) mixing chitosan, glacial acetic acid and deionized water according to a mass ratio of 5: 2: 18, heating in water bath to 80 ℃, uniformly stirring at constant temperature, adding stearic acid with the mass of 0.6 time that of the chitosan, and stirring until the stearic acid is dissolved to prepare a modified chitosan solution;
(6) soaking modified activated carbon in a modified chitosan solution, wherein the mass ratio of the modified activated carbon to the modified chitosan solution is 1: and 8, heating to 150 ℃, keeping the temperature for 30min while stirring, drying to constant weight at the stirring speed of 400rpm, and blowing at the air speed of 0.08m/s for 3min to obtain the finished product.
Comparative example 1
An oil stain absorbent mainly comprises the following components in parts by weight:
1 part of modified activated carbon and 2 parts of modified chitosan;
the preparation method of the oil stain adsorbent comprises the following steps:
(1) placing the carbonaceous material into a ball mill for ball milling for 1.5h, and sieving with a 100-mesh sieve;
(2) adding coal tar with the mass of 0.125 times that of the carbonaceous material into the screened carbonaceous material, uniformly stirring, and then pressing and forming to prepare an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment at 850 ℃, and simultaneously detecting the pressure of the closed environment until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent matrix into a potassium carbonate solution with the mass fraction of 10% to perform secondary activation in a pressure-variable closed container, wherein the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: 50, cooling to 700 ℃, wherein the cooling rate is 50 ℃/h, introducing inert gas into the potassium carbonate solution, circulating until the solution is evaporated to dryness, introducing the inert gas at a rate of 3L/h, recording the time for completely evaporating the solution to dryness, and the total circulating time is three times of the time for completely evaporating to dryness to prepare modified activated carbon;
(5) mixing chitosan, glacial acetic acid and deionized water according to a mass ratio of 5: 2: 18, heating in water bath to 80 ℃, uniformly stirring at constant temperature, adding stearic acid with the mass of 0.6 time that of the chitosan, and stirring until the stearic acid is dissolved to prepare a modified chitosan solution;
(6) soaking modified activated carbon in a modified chitosan solution, wherein the mass ratio of the modified activated carbon to the modified chitosan solution is 1: and 5, heating to 150 ℃, keeping the temperature for 20min while stirring, drying to constant weight at the stirring speed of 200rpm, and blowing at the air speed of 0.05m/s for 2min to obtain the finished product.
Comparative example 2
An oil stain absorbent mainly comprises the following components in parts by weight:
1 part of modified activated carbon and 2 parts of modified chitosan;
the preparation method of the oil stain adsorbent comprises the following steps:
(1) mixing a carbonaceous material and calcium-aluminum hydrotalcite according to a mass ratio of 8: 1, uniformly mixing to prepare a mixed material, placing the mixed material into a ball mill for ball milling, wherein the ball milling time is 1.5h, and sieving by a 100-mesh sieve;
(2) adding coal tar with the mass of 0.125 times of that of the sieved mixed material into the mixed material, uniformly stirring, and then pressing and forming to obtain an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment at 850 ℃, and simultaneously detecting the pressure of the closed environment until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent matrix into a potassium carbonate solution with the mass fraction of 10% to perform secondary activation in a pressure-variable closed container, wherein the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: 50, cooling to 700 ℃, wherein the cooling rate is 50 ℃/h, recording the complete evaporation drying time of the solution, and the total circulation time is three times of the complete evaporation drying time to prepare modified activated carbon;
(5) mixing chitosan, glacial acetic acid and deionized water according to a mass ratio of 5: 2: 18, heating in water bath to 80 ℃, uniformly stirring at constant temperature, adding stearic acid with the mass of 0.6 time that of the chitosan, and stirring until the stearic acid is dissolved to prepare a modified chitosan solution;
(6) soaking modified activated carbon in a modified chitosan solution, wherein the mass ratio of the modified activated carbon to the modified chitosan solution is 1: and 5, heating to 150 ℃, keeping the temperature for 20min while stirring, drying to constant weight at the stirring speed of 200rpm, and blowing at the air speed of 0.05m/s for 2min to obtain the finished product.
Comparative example 3
An oil stain absorbent mainly comprises the following components in parts by weight:
1 part of modified activated carbon and 2 parts of modified chitosan;
the preparation method of the oil stain adsorbent comprises the following steps:
(1) mixing a carbonaceous material and calcium-aluminum hydrotalcite according to a mass ratio of 8: 1, uniformly mixing to prepare a mixed material, placing the mixed material into a ball mill for ball milling, wherein the ball milling time is 1.5h, and sieving by a 100-mesh sieve;
(2) adding coal tar with the mass of 0.125 times of that of the sieved mixed material into the mixed material, uniformly stirring, and then pressing and forming to obtain an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment at 850 ℃, and simultaneously detecting the pressure of the closed environment until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent matrix into a potassium carbonate solution with the mass fraction of 10% to perform secondary activation in a pressure-variable closed container, wherein the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: and 50, cooling to 700 ℃, wherein the cooling rate is 50 ℃/h, introducing inert gas into the potassium carbonate solution, circulating until the solution is evaporated to dryness, introducing the inert gas at the rate of 3L/h, recording the time for completely evaporating the solution to dryness, and circulating the total time to be three times of the time for completely evaporating to dryness to prepare the finished product.
Effect example 1
Table 1 below shows the results of the oil stain adsorption performance analysis using the oil stain adsorbents of examples 1 and 2 of the present invention and comparative examples 1, 2 and 3.
TABLE 1
| Oil removal Rate (%) | |
| Example 1 | 98.9 |
| Example 2 | 99.1 |
| Comparative example 1 | 67.1 |
| Comparative example 2 | 85.3 |
| Comparative example 3 | 60.3 |
The comparison of experimental data of examples 1 and 2 and comparative examples 1, 2 and 3 shows that the oil stain absorbent prepared by the invention has a strong oil stain absorption effect, and the results show that the specific surface area can be increased and the absorption performance of the product can be further enhanced by adding calcium-aluminum hydrotalcite during preparation of an absorbent blank, performing circulating ventilation during secondary activation and immersing modified activated carbon in modified chitosan.
Effect example 2
Table 2 below shows the results of the lipophilicity analysis of the oil stain adsorbents according to examples 1 and 2 and comparative example 3.
TABLE 2
Compared with the experimental data of the comparative example 3, the experimental data of the examples 1 and 2 show that the oil stain absorbent prepared by the invention has small quality change after absorbing water, indicates that the hydrophilicity is weak, and the lipophilicity is strong, indicates that the specific surface area can be increased by soaking the modified activated carbon in the modified chitosan and blowing the modified activated carbon when preparing the product, so that the adsorption performance of the product is enhanced, and the lipophilicity of the product is enhanced.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the oil stain adsorbent is characterized in that the process flow for preparing the oil stain adsorbent is as follows: preparing an adsorbent blank, pressing and forming, primarily activating, secondarily activating, preparing modified chitosan, and preparing an oil stain adsorbent.
2. The method for preparing the oil stain absorbent according to claim 1, wherein the method for preparing the oil stain absorbent comprises the following specific steps:
(1) uniformly mixing a carbonaceous material and hydrotalcite to prepare a mixed material, placing the mixed material into a ball mill for ball milling, wherein the ball milling time is 1.5-3 h, and sieving the mixed material with a 100-mesh sieve;
(2) adding coal tar into the sieved mixed material, uniformly stirring, and then pressing and forming to obtain an adsorbent blank;
(3) preliminarily activating the adsorbent blank in a closed environment, and detecting the pressure of the closed environment at the same time until the pressure of the closed environment is stable to obtain an preliminarily activated adsorbent matrix;
(4) immediately transferring the adsorbent substrate into a potassium carbonate solution with the mass fraction of 10-30%, carrying out secondary activation in a pressure-variable closed container, cooling, introducing inert gas into the potassium carbonate solution, circulating until the solution is evaporated to dryness, recording the time for completely evaporating the solution to dryness, and obtaining modified activated carbon, wherein the total circulating time is three times of the time for completely evaporating to dryness;
(5) mixing chitosan, glacial acetic acid and deionized water according to a mass ratio of 5: 2: 18, heating in water bath to 80 ℃, uniformly stirring at constant temperature, adding stearic acid with the mass of 0.6 time that of the chitosan, and stirring until the stearic acid is dissolved to prepare a modified chitosan solution;
(6) and soaking the modified activated carbon in the modified chitosan solution, heating to 150-200 ℃, stirring while preserving heat for 20-30 min, drying to constant weight, and blowing to obtain a finished product.
3. The method for preparing the oil stain absorbent according to claim 2, wherein in the step (1): the hydrotalcite is calcium aluminum hydrotalcite; the mass ratio of the carbonaceous material to the hydrotalcite is 8: 1-10: 1.
4. the method for preparing the oil stain absorbent according to claim 2, wherein in the step (2): the mass ratio of the coal tar to the mixed material is 1: 8-1: 10.
5. the method for preparing the oil stain absorbent according to claim 2, wherein in the step (3): the primary activation temperature is 850-1100 ℃.
6. The method for preparing the oil stain absorbent according to claim 2, wherein in the step (4): the mass ratio of the adsorbent matrix to the potassium carbonate solution is 1: 50-1: 80; cooling to 700-900 ℃, wherein the cooling rate is 50 ℃/h; the inert gas is introduced at a rate of 3-5L/h.
7. The method for preparing the oil stain absorbent according to claim 2, wherein in the step (6): the mass ratio of the modified activated carbon to the modified chitosan solution is 1: 5-1: 8; the stirring speed is 200-400 rpm; the air speed is 0.05-0.08 m/s during air blowing, and the time is 2-3 min.
8. The preparation method of the oil stain absorbent according to claim 1, wherein the oil stain absorbent prepared by the preparation method of the oil stain absorbent comprises the following raw materials in parts by weight: 1-2 parts of modified activated carbon and 2-4 parts of modified chitosan.
9. The method for preparing the oil stain absorbent according to claim 8, wherein the modified activated carbon is prepared by mixing a carbonaceous material and hydrotalcite and performing primary activation and secondary activation; the modified chitosan is prepared by grafting stearic acid on chitosan.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110624339.9A CN113318709A (en) | 2021-06-04 | 2021-06-04 | Oil stain adsorbent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110624339.9A CN113318709A (en) | 2021-06-04 | 2021-06-04 | Oil stain adsorbent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113318709A true CN113318709A (en) | 2021-08-31 |
Family
ID=77419629
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110624339.9A Pending CN113318709A (en) | 2021-06-04 | 2021-06-04 | Oil stain adsorbent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113318709A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114686332A (en) * | 2022-03-28 | 2022-07-01 | 山东工大食品科技有限公司 | Decolouring and impurity removing process for new Maotai-flavor liquor |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050028624A (en) * | 2003-09-19 | 2005-03-23 | 한국전력공사 | Adsorbent for carbon dioxide fixation and method for preparing the same |
| CN104492374A (en) * | 2014-11-21 | 2015-04-08 | 合肥工业大学 | Method for preparing cerium dioxide / calcium aluminum layered di-hydroxy composite metal oxide / activated carbon composite material |
| CN105854793A (en) * | 2016-03-31 | 2016-08-17 | 烟台智本知识产权运营管理有限公司 | A preparing method of a carbon nanotube/LDHs composite material adsorbing metal ions in hyperpure ammonia |
| CN107597066A (en) * | 2017-09-18 | 2018-01-19 | 华南理工大学 | A kind of activated carbon/chitosan compound adsorbing agent and its preparation and application |
| CN109289772A (en) * | 2018-10-30 | 2019-02-01 | 蔡菁菁 | A kind of carbon nanotube/hydrotalcite material and preparation method removing nitrate nitrogen in water removal |
| CN109592679A (en) * | 2019-01-26 | 2019-04-09 | 南阳师范学院 | A kind of preparation process of sponge active carbon |
| CN110639464A (en) * | 2019-09-27 | 2020-01-03 | 湖北葛店人福药用辅料有限责任公司 | Adsorbent composition, preparation method thereof and application of adsorbent composition in refining polysorbate 80 |
| CN112239206A (en) * | 2020-11-11 | 2021-01-19 | 江苏浦士达环保科技股份有限公司 | Preparation method of low-ash pressed coal activated carbon |
| CN112456491A (en) * | 2020-11-11 | 2021-03-09 | 江苏浦士达环保科技股份有限公司 | Production process of environment-friendly regenerated activated carbon |
| CN112624405A (en) * | 2020-12-17 | 2021-04-09 | 张倩茹 | Water purifying capsule for treating oily wastewater |
-
2021
- 2021-06-04 CN CN202110624339.9A patent/CN113318709A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050028624A (en) * | 2003-09-19 | 2005-03-23 | 한국전력공사 | Adsorbent for carbon dioxide fixation and method for preparing the same |
| CN104492374A (en) * | 2014-11-21 | 2015-04-08 | 合肥工业大学 | Method for preparing cerium dioxide / calcium aluminum layered di-hydroxy composite metal oxide / activated carbon composite material |
| CN105854793A (en) * | 2016-03-31 | 2016-08-17 | 烟台智本知识产权运营管理有限公司 | A preparing method of a carbon nanotube/LDHs composite material adsorbing metal ions in hyperpure ammonia |
| CN107597066A (en) * | 2017-09-18 | 2018-01-19 | 华南理工大学 | A kind of activated carbon/chitosan compound adsorbing agent and its preparation and application |
| CN109289772A (en) * | 2018-10-30 | 2019-02-01 | 蔡菁菁 | A kind of carbon nanotube/hydrotalcite material and preparation method removing nitrate nitrogen in water removal |
| CN109592679A (en) * | 2019-01-26 | 2019-04-09 | 南阳师范学院 | A kind of preparation process of sponge active carbon |
| CN110639464A (en) * | 2019-09-27 | 2020-01-03 | 湖北葛店人福药用辅料有限责任公司 | Adsorbent composition, preparation method thereof and application of adsorbent composition in refining polysorbate 80 |
| CN112239206A (en) * | 2020-11-11 | 2021-01-19 | 江苏浦士达环保科技股份有限公司 | Preparation method of low-ash pressed coal activated carbon |
| CN112456491A (en) * | 2020-11-11 | 2021-03-09 | 江苏浦士达环保科技股份有限公司 | Production process of environment-friendly regenerated activated carbon |
| CN112624405A (en) * | 2020-12-17 | 2021-04-09 | 张倩茹 | Water purifying capsule for treating oily wastewater |
Non-Patent Citations (2)
| Title |
|---|
| S.苏珊•尼尔森 主编: "《食品分析》", 31 May 2019 * |
| 王君雅: ""类水滑石/碳基复合材料的制备及其中温吸附CO2性能研究"", 《中国优秀博硕士学位论文全文数据库（博士） 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114686332A (en) * | 2022-03-28 | 2022-07-01 | 山东工大食品科技有限公司 | Decolouring and impurity removing process for new Maotai-flavor liquor |
| CN114686332B (en) * | 2022-03-28 | 2024-01-23 | 山东工大食品科技有限公司 | Decoloring and impurity removing process for new Maotai-flavor white spirit |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zubbri et al. | Low temperature CO2 capture on biomass-derived KOH-activated hydrochar established through hydrothermal carbonization with water-soaking pre-treatment | |
| Nagy et al. | Isotherm and thermodynamic studies of Cd (II) removal process using chemically modified lignocellulosic adsorbent | |
| CN107413296B (en) | Biological carbon ferro-manganese spinel composite material for adsorbing heavy metal antimony cadmium | |
| US5614459A (en) | Process for making activated charcoal | |
| EP1103522A1 (en) | Coated activated carbon | |
| EP0554805A1 (en) | Air separation by pressure swing adsorption with a high capacity carbon molecular sieve | |
| Misran et al. | Activated carbon preparation from bagasse and banana stem at various impregnation ratio | |
| CN113318709A (en) | Oil stain adsorbent and preparation method thereof | |
| CN114570329B (en) | Preparation process and application of sludge biochar | |
| CN114029035A (en) | Preparation method of modified sludge biochar, obtained biochar and application | |
| US12064746B2 (en) | Mercury adsorbent and method for producing same | |
| CN115254027B (en) | Fibrous clay/lignin carbon porous composite material, preparation method and adsorption application | |
| CN114082403A (en) | Sulfur-based intercalated hydrotalcite-modified biochar-based adsorption material, and preparation and application thereof | |
| CN113842884A (en) | Medium-temperature hydrophobic decarbonization adsorbent and preparation method thereof | |
| CN111408343A (en) | Preparation method of three-dimensional biochar and application of three-dimensional biochar in heavy metal adsorption | |
| Xu et al. | Preparation and characterization of activated carbon from reedy grass leaves in a two-step activation procedure | |
| JP2000226207A (en) | Production of activated charcoal and activated charcoal | |
| Rwayhah et al. | Nanoporous activated carbon from olive stones wastes | |
| CN113856628B (en) | Metal modified biochar capable of efficiently recovering and desorbing phosphorus, and preparation method and application thereof | |
| CN113318699B (en) | Method for reducing composite molten salt in adsorbent by adding high-activity ions | |
| CN114471477A (en) | Three-dimensional porous chitosan/coal-based activated carbon composite sponge, preparation method thereof and application of composite sponge in extracting uranium from seawater | |
| CN112850707A (en) | Preparation method of activated carbon | |
| Hidayah et al. | Preparation and characterization of activated carbon from the sea mango (Cerbera Odollam) with impregnation in phosphoric acid (H3PO4) | |
| Li et al. | Comparative study of using different materials as bacterial carriers to treat hydrogen sulfide | |
| Suhirman et al. | Preparation of Potassium Permanganate Confined in Porous Carbon Synthesized from Palm Kernel Shell and its Application for Hydrogen Sulfide Removal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |