CN109110757B - Activated bone charcoal and preparation method thereof - Google Patents

Activated bone charcoal and preparation method thereof Download PDF

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CN109110757B
CN109110757B CN201811329401.6A CN201811329401A CN109110757B CN 109110757 B CN109110757 B CN 109110757B CN 201811329401 A CN201811329401 A CN 201811329401A CN 109110757 B CN109110757 B CN 109110757B
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李海朝
黄丽娟
杨斯乔
张净净
宋桂秀
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Qinghai Nationalities University
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
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    • C01B32/318Preparation characterised by the starting materials
    • C01B32/324Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • CCHEMISTRY; METALLURGY
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
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    • C01B32/312Preparation
    • C01B32/342Preparation characterised by non-gaseous activating agents
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    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract

The invention relates to the field of adsorption materials, and provides activated bone charcoal and a preparation method thereof. TheThe preparation method of the activated bone charcoal comprises mixing the crushed animal waste bone with activating agent and soaking for 12-20 h; and then activating for 60-90 min at the temperature of 500-850 ℃ to obtain an activated material, directly washing the activated material with water until the pH value is 6-8, and drying to obtain the activated bone charcoal. The specific surface area of the activated bone charcoal is 200-500m2The methylene blue adsorption value is 30-130 mg/g. The application is beneficial to realizing the resource utilization of various animal waste bones and saving resources such as wood, coal, coconut shells and the like. The prepared various animal bone-based activated bone charcoals can be used for replacing part of the traditional activated carbon products; the preparation process does not need inert gas protection, the process is simple, and the industrial production is easy to realize.

Description

Activated bone charcoal and preparation method thereof
Technical Field
The invention relates to the field of adsorption materials, and particularly relates to activated bone charcoal and a preparation method thereof.
Background
The carbon adsorption material is a porous carbon-containing material, has the characteristics of developed pore structure, large specific surface area and the like, is an excellent adsorbent, has stable performance, is easy to regenerate, is an environment-friendly adsorbent, and is widely applied to the directions of metallurgy, chemical industry, environmental protection and the like. At present, in the process of preparing the carbon adsorption material, substances rich in carbon-containing elements, such as wood, coal, various nut shells and the like, are mainly used as raw materials, and the preparation of various carbon adsorption materials becomes a research hotspot of scholars at home and abroad.
It is well known that China has more than 13 hundred million people, and the amount of various meat foods consumed is huge, so that the amount of various livestock and poultry waste bones generated is huge and amazing. Generally, bones account for a certain proportion of organisms, namely 12.9 percent of pigs, 20.5 percent of cows and 32.2 percent of sheep (the bone proportion of sheep is the average value of 24.3 percent of first-level sheep, 31.8 percent of second-level sheep and 40.5 percent of lean sheep), and 30 to 45 percent of poultry. Taking 2015 as an example, the meat yield of pigs, cattle, sheep and poultry is 5486.5, 700.1, 440.8 and 1826.3 ten thousand tons respectively, and further, the pig bone yield is estimated to be more than 812 ten thousand tons, the cattle bone yield is estimated to be more than 180 ten thousand tons, the sheep bone yield is estimated to be more than 209 ten thousand tons, and the poultry bone yield is estimated to be more than 782 to 1264 ten thousand tons in the current year. The treatment of the bones becomes a difficult problem, and the bad treatment pollutes the environment and wastes resources.
Disclosure of Invention
The invention aims to provide a preparation method of activated bone charcoal, which prepares various animal waste bones into an activated carbon material, well utilizes the waste bones, and is beneficial to resource recycling and environmental protection.
The invention also aims to provide the activated bone charcoal, which can replace the activated charcoal for multiple adsorption purposes, is not only beneficial to realizing resource utilization of waste such as various animal waste bones, but also beneficial to saving resources such as wood, coal, coconut shells and the like.
The embodiment of the invention is realized by the following steps:
a method for preparing activated bone charcoal comprises mixing pulverized animal waste bone with activating agent and soaking for 12-20 hr; and then activating for 60-90 min at the temperature of 500-850 ℃ to obtain an activated material, directly washing the activated material with water until the pH value is 6-8, and drying to obtain the activated bone charcoal.
An activated bone charcoal, which is prepared by the preparation method of the activated bone charcoal; the specific surface area of the activated bone charcoal is 200-500m2The methylene blue adsorption value is 30-130 mg/g.
The beneficial effects of the embodiment of the invention include:
the method takes the waste animal bones as raw materials, and phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride as an activating agent to prepare the activated bone charcoal with large specific surface area and high adsorption performance; is beneficial to realizing the resource utilization of various animal waste bones and saving resources such as wood, coal, coconut shell and the like. The prepared various animal bone-based activated bone charcoals can be used for replacing part of the traditional activated carbon products; the preparation process does not need inert gas protection, the process is simple, and the industrial production is easy to realize.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The activated bone charcoal and the method for preparing the same according to the embodiments of the present invention will be described in detail below.
The composition of bones is complex, and the composition structure and chemical components of animal bones and poultry bones are different, so that the reasonable utilization is challenged. At present, the waste bone is utilized mainly by making bone charcoal into bone paste (firstly softening at high temperature and then crushing at high power), bone glue (extracting bone marrow by high-pressure cooking, heating again, dissolving and bleaching, then concentrating in a vacuum evaporation tank, and finally drying to obtain a finished product), bone oil (crushing bones, adding water, boiling until the bones become powder, taking out oil on the surface of a pot, concentrating into bone oil), bone meal (adding water to the bone meal left after extracting the bone oil, heating a small amount of potassium carbonate for 24-30 hours, then drying, crushing and screening into bone meal), bone fat (putting the bones into a pressure pot, cooking for 10 hours, then taking out upper liquid, putting the upper liquid into a water bath, repeatedly heating, then extracting upper yellowish, transparent and anhydrous bone fat, bone ash (burning the bones of livestock and poultry till the bones become ash), bone drying (scraping the bones, soaking the inner tendons in quick lime water for 20-30 natural times, taking out, exposing to the sun, finally rubbing and repairing the bones into the bone dried bones) and obtaining the bone, then carbonizing at high temperature, taking out and crushing to obtain bone charcoal), and the products have wide application in the aspects of food, chemical industry, manufacture of articles for daily use, medicine, agricultural fertilizer and the like.
Various animal waste bones are innovatively prepared into the activated carbon material, so that the waste bones are well utilized, and the resource recycling and the environment protection are facilitated.
Specifically, the application provides a preparation method of activated bone charcoal, which comprises the following steps:
s1, airing: drying the waste animal bones until the water content is 5-15%.
S2, crushing: animal waste bones are crushed according to the process requirement.
S3, impregnation of an activating agent: mixing the crushed animal waste bone with activating agent and soaking for 12-20 h. Wherein the mass ratio of the activating agent to the waste animal bones is 1.5-3:1, and the activating agent comprises one or more of potassium hydroxide, phosphoric acid, zinc chloride and magnesium chloride.
By impregnating the waste animal bones with activating agents, the activating agents generally have dehydration and swelling effects on carbon-containing organic matters and can fully contact with the waste animal bones to activate the waste animal bones at a certain temperature (different activating agents require different temperature ranges), and the activating agents interact with materials at a high temperature in the process to fix carbon elements (such as phosphoric acid) in the organic matters, so that the amorphous parts are corroded and oxidized to form micropores and mesopores, thereby greatly increasing the specific surface area) and activating the waste animal bones into adsorbing materials with stronger adsorption capacity.
It is noted that different activators were selected with slightly different mass ratios to animal waste bone and different concentrations of activator.
For example: in other embodiments of the present application, when the activator is potassium hydroxide, the mass ratio of potassium hydroxide to animal waste bone is 1.5-2.5:1, the concentration of potassium hydroxide is greater than 50%; in other embodiments of the present application, when the activator is phosphoric acid, the mass ratio of phosphoric acid to the animal waste bone is 2-3:1, and the concentration of phosphoric acid is 50-85%; in other embodiments of the present application, when the activator is zinc chloride, the mass ratio of the zinc chloride to the animal waste bone is 2-3:1, and the concentration of the zinc chloride is greater than 60%; in other embodiments of the present application, when the activator is magnesium chloride, the mass ratio of magnesium chloride to the animal waste bone is 2-3:1, and the concentration of magnesium chloride is greater than 60%.
S4, high-temperature activation: and then activating for 60-90 min at the temperature of 500-850 ℃ to obtain the activated material.
Specifically, heating to a first activation temperature at a heating rate of 15-25 ℃/min, activating for 20-30min, heating to a second activation temperature at a heating rate of 5-10 ℃/min, and continuing to activate for 40-60 min; wherein the first activation temperature is 500-750 ℃, and the second activation temperature is 600-850 ℃; the first activation temperature is lower than the second activation temperature.
In the application, the immersed animal waste bone is subjected to high-temperature activation through the stepped activation temperature, the temperature is increased to a first activation temperature at the temperature increase speed of 15-25 ℃/min, the animal waste bone is activated at the first activation temperature, preheating and carbonization of the animal waste bone are realized, meanwhile, an activating agent attached to the surface of the animal waste bone after immersion is partially evaporated by high temperature to form gas, at the moment, part of the gas enters the inside of the carbon material along with carbonization of the animal waste bone, and after activation at the first activation temperature is finished, the temperature is increased to a second activation temperature at the temperature increase speed of 5-10 ℃/min, so that the temperature increase rate when the temperature is increased to the second activation temperature is obviously lower than that when the temperature is increased to the first activation temperature, because the temperature is increased to the first activation temperature at a higher temperature increase speed for activation, the animal waste bone is carbonized as soon as possible, and then the temperature is raised to the second activation temperature at a lower temperature raising speed, so that the carbonized animal waste bone is continuously opened in a continuous activation state, and is easy to react with gas generated by the high temperature of the activating agent, and further, the pores are continuously enlarged and develop to the depth. As the activation reaction is continuously carried out, the activation temperature is increased to the second activation temperature, new unsaturated carbon atoms or active points are exposed on the surface of the microcrystal, and then the new active points can react with other molecules of the activation gas, so that the uneven combustion on the surface of the microcrystal continuously causes the formation of new pores, and the activation effect is better.
It is noted that the activation temperatures are slightly different when different activators are used. For example: in other embodiments herein, when the activator is potassium hydroxide, the activation temperature is 750 ℃ to 850 ℃; in other embodiments herein, when the activator is phosphoric acid, zinc chloride or magnesium chloride, the activation temperature is from 500 ℃ to 600 ℃.
S5, cooling: cooling the activated material to room temperature at a cooling speed of 8-11 ℃/min. The temperature is reduced and cooled at a specific temperature reduction speed, so that the contact time of the activated material and air is reduced, the porous structure on the surface of the activated material is shaped in the temperature reduction process, the activated material is not easily influenced by oxygen, carbon dioxide or water vapor in the air, and the property of the activated material is favorably kept.
S6, water washing: directly washing the activated material with water until the pH value is 6-8.
The active material is directly washed by water instead of acid, so that the surface structure of the active material is protected to the maximum extent, and meanwhile, the active agent which does not react with the animal waste aggregate can be recycled in the washing process by water.
It is noted that when different activators are used, the pH obtained by washing the activator with water is slightly different. For example: in other embodiments herein, when the activator is potassium hydroxide, it is washed directly with water to a pH of 7-8; in other embodiments herein, when the activator is phosphoric acid, zinc chloride or magnesium chloride, it is washed directly with water to a pH of 6-7.
S7, drying: drying at 100-120 deg.C for 8-12h to obtain activated bone charcoal, and removing water on the surface of the activated bone charcoal by drying.
After drying, the yield of the activated bone charcoal can be obtained by calculating the mass percentage of the mass of the activated bone charcoal to the mass of the oven dry raw material, and the specific surface area of the activated bone charcoal obtained by the method is 200-2The methylene blue adsorption value is 30-130 mg/g.
The specific surface area of the activated bone charcoal was measured by a Tristar3000analyzer (Micromeritics, USA). The specific surface area was calculated according to the Brunaue-Emmett-Teller (BET) equation. The method for measuring the methylene blue adsorption value comprises the following steps: the methylene blue adsorption value is measured according to the national standard GB/T12496.10-1999 test method of wooden activated carbon: determination of methylene blue adsorption value.
The method takes the waste animal bones as raw materials, and phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride as an activating agent to prepare the activated bone charcoal with large specific surface area and high adsorption performance; is beneficial to realizing the resource utilization of various animal waste bones and saving resources such as wood, coal, coconut shell and the like. The prepared various animal bone-based activated bone charcoals can be used for replacing part of the traditional activated carbon products; the preparation process does not need inert gas protection, the process is simple, and the industrial production is easy to realize.
The activated bone charcoal and the preparation method thereof according to the present invention are further illustrated below with reference to examples.
Example 1
The embodiment provides an active aggregate (phosphoric acid activated waste pig bone charcoal adsorbing material), and the preparation method comprises the following steps:
20g of waste pig bone material was weighed out and mixed with 50g of phosphoric acid (85% strength) activator and immersed for 15 hours. And (3) putting the completely soaked materials into a box-type resistance furnace, heating to 550 ℃ at the speed of 20 ℃/min, activating for 60min, naturally cooling to room temperature, taking out, washing for 5 times, filtering, drying at 110 ℃ for 10h, taking out, grinding, sieving, and filling the prepared powdery activated pig bone charcoal adsorbing material sample into a sample bag for later use.
Examples 2 to 5
Examples 2 to 5 provide an active aggregate (phosphoric acid-activated waste pig bone charcoal adsorbing material) which is prepared substantially in the same manner as in example 1, except that:
in example 2, the temperature is raised to 500 ℃ at a rate of 20 ℃/min for activation for 20min, and then the temperature is raised to 600 ℃ at a rate of 10 ℃/min for continuous activation for 40 min;
in example 3, after activation, the activated material was cooled to room temperature at a cooling rate of 10 ℃/min.
In example 4, the temperature was raised to 500 ℃ at 20 ℃/min for activation for 20min, and then raised to 600 ℃ at a temperature rise rate of 10 ℃/min for further activation for 40 min; and then cooling the activated material to room temperature at a cooling speed of 10 ℃/min.
In example 5, the raw material was a waste bovine bone material.
The products obtained in the above examples 1 to 5 were tested for yield, specific surface area and methylene blue adsorption value, and comparative examples 1 to 5 were obtained by changing the activation parameters of the above example 1, while the products obtained in the above comparative examples 1 to 5 were tested for yield, specific surface area and methylene blue adsorption value, and the test results are shown in table 1.
TABLE 1 phosphoric acid activation of waste pig bone charcoal product Properties
Figure BDA0001859487710000091
As can be seen from Table 1, the amount of activator, the activation temperature and the activation time all have a relatively important influence on the activation result, and when the temperature is too high or too low, the ideal activated product cannot be obtained when the amount of activator is less than 2: 1. Meanwhile, the stepped activation temperature is set, and the activation time and the cooling rate are controlled during activation, so that the performance of the product is improved.
Example 6
The embodiment provides activated bone charcoal (potassium hydroxide activated waste pig bone charcoal), and the preparation method comprises the following steps:
weighing 20g of waste pig bone raw material, mixing with 30g of pure potassium hydroxide (prepared into 50% aqueous solution) activator, and soaking for 20 h. And (3) putting the completely soaked materials into a box-type resistance furnace, heating to 800 ℃ at a speed of 15 ℃/min, activating for 60min, cooling to room temperature, taking out, washing for 5 times, filtering, drying at 110 ℃ for 10h, taking out, grinding, sieving, and filling the prepared powdery active waste pig bone charcoal adsorbing material sample into a sample bag for later use.
Examples 7 to 10
Examples 7 to 10 provide an active aggregate (phosphoric acid-activated waste pig bone charcoal adsorbing material) which is prepared substantially in the same manner as in example 1, except that:
in example 7, the temperature was raised to 750 ℃ at 15 ℃/min for activation for 20min, and then raised to 800 ℃ at a rate of 5 ℃/min for further activation for 40 min;
in example 8, after activation, the activated material was cooled to room temperature at a cooling rate of 8 ℃/min.
In example 9, the temperature was raised to 750 ℃ at 15 ℃/min for activation for 20min, and then raised to 800 ℃ at a rate of 5 ℃/min for further activation for 40 min; and then cooling the activated material to room temperature at a cooling speed of 8 ℃/min.
In example 10, the raw material was a waste bovine bone material.
The products obtained in the above examples 7 to 10 were tested for yield, specific surface area and methylene blue adsorption value, and comparative examples 6 to 8 were obtained by changing the activation temperature of the above example 7, while the yield, specific surface area and methylene blue adsorption value of comparative examples 6 to 8 were tested, and the test results are shown in Table 2.
TABLE 2 Properties of potassium hydroxide-activated waste pig bone charcoal products
Figure BDA0001859487710000111
Example 11
The embodiment provides an activated bone charcoal (zinc chloride activated waste pig bone charcoal adsorbing material), and the preparation method comprises the following steps:
20g of waste pig bone raw material is weighed and mixed with 60g of pure zinc chloride (prepared into an aqueous solution with the concentration of 60%) activating agent, and the mixture is soaked for 24 hours. And (3) putting the completely soaked materials into a box-type resistance furnace, heating to 500 ℃ at a speed of 20 ℃/min, activating for 90min, cooling to room temperature, taking out, washing for 5 times, filtering, drying at 110 ℃ for 10h, taking out, grinding, sieving, and filling the prepared powdery active waste pig bone charcoal adsorbing material sample into a sample bag for later use.
Examples 12 to 15
Examples 12 to 15 provide an active aggregate (zinc chloride activated waste pig bone charcoal adsorbing material) which is prepared by the method substantially the same as that of example 1, except that:
in example 12, the temperature was raised to 500 ℃ at 25 ℃/min for activation for 30min, and then the temperature was raised to 600 ℃ at a temperature rise rate of 15 ℃/min, and activation was continued for 60 min;
in example 13, after activation, the activated material was cooled to room temperature at a cooling rate of 11 ℃/min.
In example 14, the temperature was raised to 500 ℃ at 25 ℃/min for activation for 30min, and then the temperature was raised to 600 ℃ at a temperature rise rate of 15 ℃/min, and activation was continued for 60 min; and then cooling the activated material to room temperature at a cooling speed of 11 ℃/min.
In example 15, the raw material was a waste bovine bone raw material.
The products obtained in the above examples 11 to 15 were tested for yield, specific surface area and methylene blue adsorption value, and comparative examples 9 to 12 were obtained by changing the activation parameters of the above example 11, while the products obtained in comparative examples 9 to 12 were tested for yield, specific surface area and methylene blue adsorption value, and the test results are shown in Table 3.
TABLE 3 Properties of charcoal products of waste pig bones activated with zinc chloride
Figure BDA0001859487710000121
Example 16
The embodiment provides an activated bone charcoal (magnesium chloride activated waste pig bone charcoal), and the preparation method comprises the following steps:
20g of waste pig bone raw material is weighed and mixed with 60g of pure magnesium chloride (prepared into an aqueous solution with the concentration of 60%) activating agent, and the mixture is soaked for 24 hours. And (3) putting the completely soaked materials into a box-type resistance furnace, heating to 500 ℃ at the speed of 20 ℃/min, activating for 90min, cooling to room temperature, taking out, washing for 5 times, filtering, drying at the temperature of 110 ℃ for 10h, taking out, grinding, sieving, and filling the prepared powdery active waste pig bone charcoal sample into a sample bag for later use.
Examples 17 to 20
Examples 17 to 20 provide an active aggregate (phosphoric acid-activated waste pig bone charcoal adsorbing material) which is prepared substantially in the same manner as in example 1, except that:
in example 17, the temperature was raised to 500 ℃ at 20 ℃/min for activation for 30min, and then the temperature was raised to 600 ℃ at a temperature rise rate of 10 ℃/min, and activation was continued for 60 min;
in example 18, after activation, the activated material was cooled to room temperature at a cooling rate of 9 ℃/min.
In example 19, the temperature was raised to 500 ℃ at 20 ℃/min for activation for 30min, and then the temperature was raised to 600 ℃ at a temperature rise rate of 10 ℃/min, and activation was continued for 60 min; and then cooling the activated material to room temperature at a cooling speed of 9 ℃/min.
In example 20, the raw material was a waste bovine bone material.
The products obtained in the above examples 16 to 20 were tested for yield, specific surface area and methylene blue adsorption value, and comparative examples 13 to 16 were obtained by changing the activation parameters of the above example 16, while the products obtained in the comparative examples 13 to 16 were tested for yield, specific surface area and methylene blue adsorption value, and the test results are shown in Table 4.
TABLE 4 Properties of waste pig bone charcoal product activated by zinc chloride
Figure BDA0001859487710000141
Examples of the experiments
First, adsorption decolorization and heavy metal adsorption experiment of activated bone charcoal
The above examples 1 to 20 and comparative examples 1 to 16 were subjected to adsorption and desorption experiments and heavy metal adsorption experiments, respectively.
(1) The adsorption decoloration is detected by adopting the following method:
methyl orange is a typical dye. In this experiment, the activated pig bone charcoal adsorbing material prepared in example 1-3 was used to treat wastewater containing methyl orange (containing 80mg/L methyl orange). Accurately weighing 0.1g of activated bone charcoal into a 250mL conical flask at room temperature under a neutral condition, and adding 100mL of methyl orange solution with the initial mass concentration of 100 mg/L. Oscillating for 30min, standing, centrifuging, taking supernatant, measuring absorbance at maximum wavelength by a spectrophotometer, and calculating the solution concentration of the supernatant. The above experiment was repeated 3 times, and the adsorption amount (q) was calculated by the following formula.
q=(C0-Ct)V/W
In the formula: c0: the initial mass concentration of the solution, mg/L;
Ct: the mass concentration of the supernatant at the time t is mg/L;
w: mass of adsorbent, g;
v: volume of dye solution, L.
(2) The heavy metal adsorption experiment adopts the following method for detection:
the amount of industrial wastewater containing heavy metal ions such as zinc, mercury, chromium, lead and the like discharged from countries around the world every year is huge, and the adsorption method is one of effective treatment methods. Taking chromium ions Cr (VI) as an experimental object, and preparing a potassium dichromate solution with a required concentration. The solution with the chromium ion concentration of 5mg/L is put into a 250mL conical flask and adsorbed for 12h in a constant temperature oscillator at room temperature by using 1g of active bovine bone charcoal adsorbing material. Sampling, measuring the absorbance of the sample, and calculating the adsorption amount.
TABLE 5 decolorization effect and Cr (VI) adsorption effect of activated bone charcoal adsorbent
Figure BDA0001859487710000151
Figure BDA0001859487710000161
Experiments prove that various activators such as phosphoric acid, potassium hydroxide and the like have lower activation temperature (lower than 400 ℃); the waste bones of various animals are activated under the conditions of low addition amount (the mass ratio of the activating agent to the raw materials is less than 1: 1) and short activation time (less than 30min), and products with good adsorption performance (the specific surface area is less than 75 m) cannot be obtained2Methylene blue adsorption is lower than 20mg/g) and only bone charcoal is called as bone charcoal instead of activated bone charcoal.
The method takes the waste animal bones as raw materials, and phosphoric acid or potassium hydroxide or zinc chloride or magnesium chloride as an activating agent to prepare the activated bone charcoal with large specific surface area and high adsorption performance; is beneficial to realizing the resource utilization of various animal waste bones and saving resources such as wood, coal, coconut shell and the like. The prepared various animal bone-based activated bone charcoals can be used for replacing part of the traditional activated carbon products; the preparation process does not need inert gas protection, the process is simple, and the industrial production is easy to realize.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. 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 (7)

1. A preparation method of activated bone charcoal is characterized in that the preparation method comprises the steps of mixing crushed animal waste bone with an activating agent and soaking for 12-20 h; then activating for 60-90 min at the temperature of 500-850 ℃ to obtain an activated material, directly washing the activated material with water until the pH value is 6-8, and drying to obtain activated bone charcoal;
the mass ratio of the activating agent to the waste animal bones is 1.5-3: 1;
the activator comprises one or more of potassium hydroxide, phosphoric acid, zinc chloride and magnesium chloride;
activating for 60-90 min at the temperature of 500-850 ℃ to obtain an activated material, wherein the activated material comprises: heating to a first activation temperature at a heating rate of 15-25 ℃/min, activating for 20-30min, heating to a second activation temperature at a heating rate of 5-10 ℃/min, and continuing to activate for 40-60 min;
wherein the first activation temperature is 500-750 ℃, and the second activation temperature is 600-850 ℃; the first activation temperature is lower than the second activation temperature.
2. The method for preparing activated bone charcoal according to claim 1, wherein when the activating agent is potassium hydroxide, the mass ratio of the potassium hydroxide to the animal waste bone is 1.5-2.5:1, and the activation temperature is 750-850 ℃; directly washing with water to pH 7-8, wherein the concentration of potassium hydroxide is more than 50%.
3. The method for preparing activated bone charcoal according to claim 1, wherein when the activating agent is phosphoric acid, zinc chloride or magnesium chloride, the mass ratio of the phosphoric acid, the zinc chloride or the magnesium chloride to the animal waste bone is 2-3:1, and the activation temperature is 500-600 ℃; directly washing with water until the pH value is 6-7, wherein the concentration of phosphoric acid is 50-85%;
the concentration of the zinc chloride is more than 60 percent;
the concentration of the magnesium chloride is more than 60%.
4. The method of claim 1, further comprising cooling the activated material to room temperature at a cooling rate of 8-11 ℃/min after obtaining the activated material and before washing the activated material with water.
5. The method for preparing activated bone charcoal according to claim 1, wherein the activated bone charcoal is obtained by directly washing the activating material with water to pH 6-8 and then drying at 100-120 ℃ for 8-12 h.
6. The method of preparing activated bone char according to claim 1, wherein the waste animal bone is dried to a moisture content of 5-15% before being pulverized.
7. An activated bone char produced by the method for producing an activated bone char according to any one of claims 1 to 6; the specific surface area of the activated bone charcoal is 200-500m2The methylene blue adsorption value is 30-130 mg/g.
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CN109850893A (en) * 2019-01-27 2019-06-07 合肥学院 A kind of preparation method and application of ox bone active carbon
CN110918052A (en) * 2019-10-28 2020-03-27 安徽省通源环境节能股份有限公司 Preparation process of magnetic livestock bone carbonized particle adsorbent
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