CN108658071B - Biomass porous carbon taking chromium skin as raw material and preparation method and application thereof - Google Patents
Biomass porous carbon taking chromium skin as raw material and preparation method and application thereof Download PDFInfo
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- CN108658071B CN108658071B CN201710207416.4A CN201710207416A CN108658071B CN 108658071 B CN108658071 B CN 108658071B CN 201710207416 A CN201710207416 A CN 201710207416A CN 108658071 B CN108658071 B CN 108658071B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—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
- 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
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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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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Abstract
The invention relates to biomass porous carbon taking chrome skin as a raw material and a preparation method and application thereof. The method is applied to the purification of sewage containing chromium and dye by utilizing the high specific surface area, abundant pore structures and the action of metal oxides of the porous carbon.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to biomass porous carbon taking chromium skin as a raw material, and a preparation method and application thereof.
Background
The porous carbon has unique physical characteristics, has the advantages of good adsorption performance, mechanical strength, surface characteristics and the like, is an excellent adsorption material, is widely applied to the fields of environmental protection and chemical engineering, shows good application prospects in the fields of liquid phase adsorption, gas phase adsorption, energy storage materials, lithium ion batteries, lithium sulfur batteries, biosensors, catalysts, catalyst carriers and the like, and is a research hotspot of the current carbon materials.
The raw materials for preparing the porous carbon are very wide and mainly comprise mineral raw materials, synthetic polymer materials, waste polymer materials, biomass materials and the like. The mineral raw materials have the advantages of stable source, low cost, mature preparation method and the like, and are the main raw materials for preparing the porous carbon at present. In order to further reduce the achievement, reduce the dependence of mineral sources, particularly effectively utilize industrial and agricultural wastes and achieve the purpose of treating the wastes with the wastes, the preparation of porous carbon by taking biomass materials as raw materials is a research hotspot, such as rice husks, corncobs, bamboos, fruit shells, fruit pits, bagasse, animal skins, bones and the like.
The leather-making waste leather is the leftover after tanning leather in leather factories, is commonly called as 'chrome leather', is rich in collagen, can be used for producing industrial gelatin, and has very low price compared with edible gelatin and medicinal gelatin. However, its chromium content is high, and its use in the fields of food and medicine is strictly prohibited. How to guide the leather rich in collagen and chromium can effectively utilize resources, correctly guide the market development direction and realize the maximum benefit is an important research subject.
Chinese patent CN104588388.A discloses a comprehensive utilization method of chromium-containing leather waste, which solves the problem that the chromium-containing leather waste can not be fully utilized in the prior art. The method comprises the following steps: (1) shredding the chromium-containing leather waste; (2) drying the shredded chromium-containing leather waste chips; (3) carrying out high-temperature combustion on the dried chromium-containing leather waste fragments; (4) extracting chromium oxide from leather ash of the chromium-containing leather waste after high-temperature combustion. By the design scheme, the chromium-containing leather waste can be combusted, the heat energy of the chromium-containing leather waste can be utilized, and chromium in the chromium-containing leather waste can be recycled, so that the chromium-containing leather waste can be fully utilized. However, the method of the patent does not fully utilize the abundant collagen and active carbon resources in the chrome skin.
Chinese patent CN103145126.A discloses a method for preparing activated carbon by using waste leather as a raw material through a microwave method, which realizes resource recycling, has high preparation speed and simple process, and the prepared activated carbon has good adsorption effect, and comprises the following steps: (1) washing with water to remove impurities, drying, crushing, and preparing into leather particles; (2) soaking the leather particles in acid for a period of time; (3) placing the mixture in a microwave oven for carbonization and activation; (4) boiling in acid, washing to neutrality, and oven drying to obtain the leather activated carbon. However, the patent method adopts a microwave method to prepare the porous carbon, and the specific surface area of the porous carbon is 638.24-639.52m2(ii) in terms of/g. However, the specific surface area of the porous carbon prepared in the patent is not higher than that of the active carbon reported in the literatureHas the advantages of not utilizing the abundant chromium resource in the chromium skin.
Abundant carbon sources and chromium sources in the leather waste are fully utilized, waste resources are effectively utilized, and the method has important significance for solving the problems of environmental pollution and food and drug safety. According to the search, no report about the preparation of the chromium-rich activated carbon by using the chromium skin and the specific application of the activated carbon is found at present.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention utilizes tanning waste chrome skin as a raw material, and the raw material is carbonized and activated to prepare the biomass porous carbon material. The method is applied to the purification of chromium-containing sewage and the purification of methylene blue dye-containing sewage by utilizing the high specific surface area, rich pore structures and the action of metal oxides of the porous carbon.
The invention adopts the following technical scheme: the biomass porous carbon taking the chromium skin as the raw material is prepared by the following steps:
(1) a pretreatment step: drying and crushing the leather-making waste leather (chrome leather), and heating to remove grease to obtain a chrome leather pretreatment product;
(2) pre-carbonization: pre-carbonizing the chrome skin pretreatment product to obtain a chrome skin pre-carbonization product;
(3) carbonization and activation: and mixing the chromium skin pre-carbonization product with an activating agent, carbonizing and activating, washing with water, and drying to obtain the chromium skin-based porous carbon.
In a preferred embodiment of the invention, in the step (1), the tannery waste leather (chrome leather) is naturally dried, crushed to about 0.5cm × 0.5cm, heated to remove grease until no smoke is generated, and a chrome leather pretreatment product is obtained.
In a preferred embodiment of the present invention, in step (2), the chrome skin pretreatment product is placed in a tubular electric furnace in N2Or CO2Under the protection of gas, pre-carbonizing at 400-600 ℃ for 0.5-3 h to obtain a chromium skin pre-carbonized product.
In a preferred embodiment of the invention, in the step (3), the chrome skin pre-carbonization product and the activating agent are mixed according to a ratio of carbon/activating agent =3: 1-1: 3, carbonization and activation are carried out for 0.5-3 h at 600-1000 ℃, then washing is carried out until the mixture is neutral, and drying is carried out at 105-120 ℃ to obtain the chrome skin based porous carbon.
In a preferred embodiment of the present invention, in step (1), the heating temperature is controlled to 200 ℃ or less, preferably 160 ℃ or less.
In a preferred embodiment of the present invention, in the step (2), the protective gas is N2The pre-carbonization temperature is 500 ℃, and the pre-carbonization time is 1-2 h.
In a preferred embodiment of the present invention, in the step (3), the activating agent is KOH, the carbon/activating agent is 2:1 to 1:2, the carbonization temperature is 650 to 850 ℃, the carbonization time is 1 to 2 hours, and the drying temperature is 105 to 110 ℃.
On the other hand, the invention also protects the application of the biomass porous carbon in treating hexavalent chromium-containing sewage.
On the other hand, the invention also protects the application of the biomass porous carbon in treating sewage containing methylene blue dye.
Compared with the prior art, the invention has the advantages that:
(1) the preparation method of the biomass carbon with the chrome skin as the raw material has the advantages of low cost, scientific and reasonable process and easy operation, prepares the chrome skin-based porous carbon with the tanning waste chrome skin as the raw material, fully recycles the carbon resource and the chromium resource in the chrome skin, and is beneficial to comprehensive recycling and new application excavation of the chrome skin.
(2) The prepared biomass porous carbon taking the chromium skin as the raw material is applied to the fields of hexavalent chromium-containing sewage treatment and methylene blue dye-containing sewage treatment. The porous carbon material with adsorption selectivity and high specific surface area is prepared by utilizing rich carbon sources, and the prepared active carbon has developed pores and the specific surface area of more than 2000 m2The adsorption effect of the hexavalent chromium-containing sewage is superior to that of commercial activated carbon; realizes the comprehensive recycling of the chrome skin.
Drawings
FIG. 1 is an electron micrograph of a chromium skin-based porous carbon prepared under carbonization conditions at 750 ℃;
FIG. 2 shows a process for preparing a polycarbonate resin by carbonizing at 750 deg.CPore size distribution and N of prepared chrome skin-based porous carbon2An adsorption-desorption curve;
FIG. 3 is an electron micrograph of a chromium skin-based porous carbon prepared under carbonization conditions at 650 ℃;
FIG. 4 shows the pore size distribution and N of the chromium skin-based porous carbon prepared under the carbonization condition at 650 deg.C2Adsorption-desorption curve.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the invention is not limited thereto.
Example 1
(1) A pretreatment step: naturally drying the leather-making waste leather (chrome leather), crushing to about 0.5cm multiplied by 0.5cm, heating on an electric furnace to remove grease until no smoke is generated, and obtaining the chrome leather pretreatment product.
(2) Pre-carbonization: the chrome skin pretreatment product was placed in a tubular electric furnace in N2Under the protection, pre-carbonizing at 500 ℃ for 1h to obtain a chrome skin pre-carbonized product.
(3) Carbonization and activation: mixing the chrome skin pre-carbonization product with KOH according to the ratio of carbon/activating agent =1:1, carrying out carbonization and activation for 1h at 750 ℃, then washing to be neutral, and drying at 110 ℃ to obtain the chrome skin based porous carbon.
The obtained chrome skin-based porous carbon has electron micrograph shown in FIG. 1, pore size distribution and N2As shown in FIG. 2, the adsorption-desorption curve shows that the prepared chromium skin-based activated porous carbon has a hierarchical pore structure and a large specific surface area (greater than 2000 m)2/g）。
Example 2
(1) A pretreatment step: naturally drying the leather-making waste leather (chrome leather), crushing to about 0.5cm multiplied by 0.5cm, heating on an electric furnace to remove grease until no smoke is generated, and obtaining the chrome leather pretreatment product.
(2) Pre-carbonization: the chrome skin pretreatment product was placed in a tubular electric furnace in N2Under the protection, pre-carbonizing at 500 ℃ for 2h to obtain a chrome skin pre-carbonized product.
(3) Carbonization and activation: mixing the chrome skin pre-carbonization product with KOH according to the ratio of carbon/activating agent =1:1, carrying out carbonization and activation for 1h at 650 ℃, then washing to be neutral, and drying at 110 ℃ to obtain the chrome skin based porous carbon.
The obtained chrome skin-based porous carbon has an electron micrograph shown in FIG. 3, a distribution of pore diameters and N2The adsorption-desorption curve is shown in fig. 4, and the results show that the prepared chrome skin-based porous carbon has a hierarchical pore structure and a large specific surface area.
Example 3
The chromium skin-based porous carbon is used for purifying the sewage containing hexavalent chromium.
(1) Preparing Cr (VI) solution with initial pH value of 2.0 and different initial concentrations (100-700 mg/L), wherein the dosage of the chromium skin-based porous carbon is 1.0 g/L.
(2) Static adsorption experiments were performed in a thermostatic waterbath shaker (temperature 30 ℃, shaking speed 130 r/min), and after 24h the supernatant was taken to measure the remaining Cr (VI) concentration.
(3) Through a Langmuir adsorption isothermal model, the maximum adsorption capacity of the chromium-based skin-based porous carbon to hexavalent chromium at 30 ℃ is about 400 mg/g.
Example 4
The chromium skin-based porous carbon is used for purifying sewage containing methylene blue dye.
(1) Preparing methylene blue solution with initial pH value of 7.0 and different initial concentrations (100-800 mg/L), wherein the dosage of the chrome skin based porous carbon is 1.0 g/L.
(2) Static adsorption experiments were performed in a thermostatic waterbath shaker (temperature 30 ℃, shaking speed 130 r/min), and after 24h the supernatant was taken to measure the remaining Cr (VI) concentration.
(3) Through a Langmuir adsorption isothermal model, the maximum adsorption amount of the chromium-based leather porous carbon to the methylene blue dye at 30 ℃ is 565 mg/g.
While the present invention has been described with reference to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. The application of biomass porous carbon taking chromium skin as a raw material in treating hexavalent chromium-containing sewage is characterized by being prepared through the following steps:
(1) a pretreatment step: drying and crushing the chrome skin, and heating to remove grease to obtain a chrome skin pretreatment product;
(2) pre-carbonization: pre-carbonizing the chrome skin pretreatment product to obtain a chrome skin pre-carbonization product;
(3) carbonization and activation: mixing the chrome skin pre-carbonization product with an activating agent, carbonizing and activating, washing with water, and drying to obtain chrome skin-based porous carbon;
in the step (1), naturally drying the chrome skin, crushing to 0.5cm multiplied by 0.5cm, heating to remove grease until no smoke is generated, and obtaining a chrome skin pretreatment product; the heating temperature is controlled below 200 ℃;
in the step (2), the chrome skin pretreatment product is placed in a tubular electric furnace in N2Or CO2Under the protection of gas, pre-carbonizing at 400-600 ℃ for 0.5-3 h to obtain a chromium skin pre-carbonization product;
in the step (3), the chrome skin pre-carbonization product and an activating agent are mixed according to the ratio of carbon/activating agent =3: 1-1: 3, carbonization and activation are carried out for 0.5-3 h at 600-1000 ℃, then the mixture is washed to be neutral, and the mixture is dried at 105-120 ℃ to obtain the chrome skin based porous carbon.
2. Use according to claim 1, wherein in step (1), the heating temperature is controlled below 160 ℃.
3. The use of claim 1, wherein in step (2), the shielding gas is N2The pre-carbonization temperature is 500 ℃, and the pre-carbonization time is 1-2 h.
4. The use of claim 1, wherein in the step (3), the activating agent is KOH, the carbon/activating agent is 2: 1-1: 2, the carbonization temperature is 650-850 ℃, the carbonization time is 1-2 h, and the drying temperature is 105-110 ℃.
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| CN109678134A (en) * | 2019-01-25 | 2019-04-26 | 齐鲁工业大学 | A method of porous carbon materials are prepared using the waste in aldehyde-plant combination tannage process hides |
| CN110217789B (en) * | 2019-06-10 | 2021-04-09 | 陕西科技大学 | Leather-based capacitance carbon material and preparation method and application thereof |
| CN112221465B (en) * | 2020-09-10 | 2021-07-16 | 昆明理工大学 | Method for preparing porous biochar through waste-free biological refining and application |
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