CN112645323B - Preparation method of cocklebur fruit shell based biomass charcoal adsorbent and application of cocklebur fruit shell based biomass charcoal adsorbent in adsorption of radioactive radon gas - Google Patents

Preparation method of cocklebur fruit shell based biomass charcoal adsorbent and application of cocklebur fruit shell based biomass charcoal adsorbent in adsorption of radioactive radon gas Download PDF

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CN112645323B
CN112645323B CN202011328278.3A CN202011328278A CN112645323B CN 112645323 B CN112645323 B CN 112645323B CN 202011328278 A CN202011328278 A CN 202011328278A CN 112645323 B CN112645323 B CN 112645323B
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based biomass
biomass charcoal
xanthium
fruit shell
shell
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CN112645323A (en
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貟朝乐
梁珺成
周洋
罗学刚
李琛
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Southwest University of Science and Technology
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
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    • C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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    • 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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    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3441—Regeneration or reactivation by electric current, ultrasound or irradiation, e.g. electromagnetic radiation such as X-rays, UV, light, microwaves
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    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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    • C01—INORGANIC CHEMISTRY
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/02—Treating gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss

Abstract

The invention discloses a preparation method of a cocklebur fruit shell based biomass charcoal adsorbent and application of the cocklebur fruit shell based biomass charcoal adsorbent in adsorption of radioactive radon gas, wherein the preparation method comprises the following steps: cleaning the cocklebur fruit shells to remove impurities, heating to 450-550 ℃ under the protection of inert gas for carbonization for 0.5-1.5 hours, and naturally cooling to obtain a carbonized material; fully mixing the carbonized material and an activating agent according to a weight ratio of 1-10: 1-3, activating for 1-3 hours at 600-800 ℃ under the protection of inert gas, naturally cooling, soaking for 4-6 hours with a dilute hydrochloric acid solution, filtering, washing with deionized water until the filtrate is neutral, and drying to obtain the xanthium fruit shell-based biomass carbon material. The cocklebur fruit shell based biomass charcoal adsorbent material prepared by the invention has a high specific surface area and a rich micro-nano structure, has excellent adsorption performance on radioactive harmful radon gas, and can realize regeneration of the adsorption performance through simple microwave heating, high-temperature heating and other modes.

Description

Preparation method of cocklebur fruit shell based biomass charcoal adsorbent and application of cocklebur fruit shell based biomass charcoal adsorbent in adsorption of radioactive radon gas
Technical Field
The invention belongs to the fields of biomass charcoal adsorption materials and radioactive gas pollution treatment, and particularly relates to a preparation method of a cocklebur fruit shell based biomass charcoal adsorbent and application of the cocklebur fruit shell based biomass charcoal adsorbent in adsorption of radioactive radon gas.
Background
Radon gas is the only gas with a half-life of 3.8235 days, which is composed of all radioactive isotopes under normal conditions, and is released from uranium-containing minerals in rocks and soil continuously. High-concentration radon gas is often accumulated in environments such as underground position, underground engineering, the floor close to the ground in a mountain city type urban low concave area, basements, mine mining and metallurgy, rocks, building material use and the like, and health hazards are caused to workers. It has been reported that in enclosed spaces such as underground mines or houses, radon gas produces an ionizing radiation dose of about 52% of the ionizing radiation dose received by individuals. Epidemiological studies provide substantial evidence that radon exposure in the room can lead to even relatively low radon levelsLung cancer. Radon is considered to be the first cause of lung cancer in non-smokers, the second leading cancer factor in smokers. The world health organization ranks radon as one of 19 main environmental carcinogens and recommends to treat the indoor environment222Reference level of Rn is represented by current 200Bqm-3Down to 100Bqm-3。
At present, there are three methods for reducing radon at home and abroad, such as precipitation reduction, ventilation dilution and adsorption enrichment. Spraying a radon-proof coating on building materials, floors or walls with high radon exhalation rate so as to block the release of radon, but the long-term effectiveness of sealing cannot be ensured; the indoor radon concentration can be effectively reduced by increasing the air circulation and diluting the indoor radon concentration, but the energy consumption is higher and the operation is independently larger in the underground closed space; the radon concentration in a room can be reduced by activated carbon adsorption enrichment, a fiber filtration purification technology, a biological filtration technology, an electrostatic dust removal technology and the like, wherein the activated carbon adsorption enrichment is the most and most effective method currently used. However, the performance of the radon-removing activated carbon currently adopted still cannot meet the requirement, so that the device is oversize and complicated, and the cost is high. Therefore, the search for a new active carbon material with low price and good performance has important research significance.
The xanthium sibiricum is an annual herbaceous plant, has strong adaptability to the environment, can endure saline-alkali and frequent waterlogging environment for a long time, and is widely distributed in various places of China as weeds. Researches show that cocklebur fruit shells have abundant micro-nano honeycomb-shaped pore channels for transporting water and inorganic salt, biomass charcoal prepared by pyrolysis can be used as a transmission channel of harmful radioactive gas radon, a large number of micropores smaller than 2nm are prepared on the walls of the honeycomb-shaped pore channels by a physical and chemical method for modification, and the micropores can be used as adsorption sites of the radon gas.
Disclosure of Invention
The invention aims to provide a preparation method of a cocklebur fruit shell based biomass charcoal adsorbent and application thereof in radioactive harmful gas radon gas treatment by taking cocklebur fruit shells with low cost and rich resources as raw materials, so as to further reduce the cost of radon gas treatment. The cocklebur fruit shell-based biomass charcoal adsorbent prepared by the invention has higher specific surface area and better radon gas adsorption performance, and has important significance for increasing the economic added value and sustainable utilization of cocklebur and treating radioactive harmful gas radon gas.
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a xanthium shell-based biochar material, comprising the steps of:
cleaning cocklebur fruit shells to remove impurities, heating at 450-550 ℃ under the protection of inert gas for carbonization for 0.5-1.5 hours, and naturally cooling to obtain a carbonized material;
and step two, fully mixing the carbonized material and an activating agent according to the weight ratio of 1-10: 1-3, activating for 1-3 hours at 600-800 ℃ under the protection of inert gas, naturally cooling, soaking for 4-6 hours by using a dilute hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium shell-based biomass carbon material.
Preferably, the inert gas is nitrogen, and the activating agent is KOH or K2CO3And K2SiO3One or any combination of two or more of them.
Preferably, the concentration of the dilute hydrochloric acid solution is 0.08-0.12 mol/L.
Preferably, in the first step, before carbonization, the following pretreatment is further performed on the xanthium fruit shell: drying the cleaned cocklebur fruit shells at 80-100 ℃, then crushing, uniformly mixing 20-30 parts of crushed cocklebur fruit shells, 1-2 parts of sodium polyacrylate, 0.5-0.8 part of polyvinyl alcohol, 1-2 parts of sodium bicarbonate and 0.5-0.8 part of glucosamine according to parts by weight to obtain a mixture, then adding the mixture into a ball milling tank of a low-temperature stirring ball mill, adding zirconia milling balls, and carrying out ball milling by using liquid nitrogen as a ball milling medium to obtain ball milling materials, namely the pretreated cocklebur fruit shells; the liquid nitrogen filling rate in the ball milling tank is 80% -85%, the rotating speed of the stirring ball mill is 300-450 r/min, and the weight ratio of the zirconia grinding balls to the mixture is 8-10: 1, the ball milling time is 5-6 h.
Preferably, in the second step, the process of fully mixing the carbonized material and the activating agent according to the weight ratio of 1-10: 1-3 is as follows: adding the carbonized material and an activating agent into a hydrothermal reaction kettle, adding deionized water, sealing the hydrothermal reaction kettle, heating and reacting at 365-375 ℃ and 20-24 MPa for 45-60 min, cooling, and filtering; the weight ratio of the carbonized material to the deionized water is 1: 30-50.
Preferably, in the second step, in the process of soaking with the dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the process parameters are as follows: stopping ultrasound for 3-5 min at intervals after every 10-15 min of ultrasound reaction, wherein the total ultrasound time is 2-3 h, the pressure is 15-22 MPa, and the frequency is 300-450 kHz.
The invention also provides a method for preparing the cocklebur fruit shell based biomass charcoal adsorbent by adopting the cocklebur fruit shell based biomass charcoal material, which comprises the following steps:
step A, adding 80-120 parts by weight of xanthium-based biomass charcoal material into a sludge mixer, then adding 2-4 parts by weight of oleic acid and 25-35 parts by weight of plasticizing binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2-3 days;
b, adding the aged mixture into a vacuum pugging machine for vacuum pugging for 3-4 times, wherein each time lasts for 45-60 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; placing the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60-80 ℃; the pressure for extrusion molding is 10-20 MPa;
d, calcining the dried product at 600-800 ℃ for 2-3 hours; then heating to 850-900 ℃, introducing carbon dioxide, activating for 3-5 hours, and naturally cooling to obtain the xanthium sibiricum-based biomass charcoal adsorbent; the carbon dioxide was introduced at a rate of 200 sccm.
Preferably, the preparation method of the plasticized binder comprises the following steps: according to parts by weight, 1-5 parts of water-soluble starch, 2-6 parts of trehalose, 1-2 parts of mannitol, 0.5-0.8 part of polyvinylpyrrolidone and 0.3-0.5 part of polyethyleneimine are added into 20-23 parts of water, and the mixture is stirred for 30-45 min at the speed of 100-300 r/min to obtain the plasticized binder.
The invention also provides application of the cocklebur fruit shell based biomass charcoal material prepared by the preparation method in adsorption of radioactive radon gas in atmospheric environment, radioactive radon gas in underground closed space of uranium tailing area, radioactive radon gas in household residence and radioactive radon gas in office.
The invention also provides application of the cocklebur fruit shell based biomass charcoal adsorbent prepared according to the preparation method in adsorption of radioactive radon gas in an atmospheric environment, radioactive radon gas in a underground closed space of a uranium tailing area, radioactive radon gas in a household house and radioactive radon gas in an office place.
The invention at least comprises the following beneficial effects: the xanthium sibiricum is a common field weed, can be cultivated manually, has low requirement on growth conditions, is rich in resources and is low in price. The xanthium sibiricum contains a large amount of biomacromolecule substances with special structures rich in carbon elements, such as cellulose, hemicellulose, lignin and the like, has a very regular micro-nano structure, and is particularly suitable for preparing porous biomass carbon adsorbent materials and adsorbing and enriching gas. The cocklebur fruit shell based biomass charcoal adsorbent material prepared by the invention has a high specific surface area and a rich micro-nano structure, has excellent adsorption performance on radioactive harmful radon gas, and can realize regeneration of the adsorption performance through simple microwave heating, high-temperature heating and other modes.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is a scanning electron microscope image of a xanthium sibiricum shell-based biomass charcoal material prepared in example 1 of the present invention;
FIG. 2 is an XRD spectrum of a xanthium fruit shell-based biomass charcoal material prepared in example 1 of the present invention;
FIG. 3 is a gamma-ray counting chart of the xanthium fruit shell based biomass charcoal material prepared in example 1 of the present invention after radon absorption and desorption;
FIG. 4 is a graph showing the effect of adsorption-regeneration cycle of radon gas by cocklebur fruit shell based biomass charcoal material prepared in example 1 of the present invention;
FIG. 5 is a graph showing adsorption and desorption curves of xanthium sibiricum shell-based biomass charcoal material measured by a BET method;
fig. 6 is a pore size distribution diagram of the xanthium fruit shell-based biomass charcoal material.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The principle of measuring the adsorption of the cocklebur fruit shell based biomass charcoal material to radioactive radon gas is as follows: the decay daughter lead-214 and bismuth-214 of radon can generate characteristic gamma rays in the decay process, the gamma peaks of lead-214 are 242, 294 and 352KeV, and the gamma peak of bismuth-214 is 609 KeV. When radon reaches radioactive equilibrium with its decay daughter, the adsorption performance of carbon materials to radon can be described by measuring the characteristic gamma count or gamma ray peak (or peak cluster) area of the radon daughter. In the measurement process, the radon absorption performance of the material can be determined by gamma total counting by taking commercial activated carbon as a contrast under the condition that all conditions are consistent.
The radon adsorption measurement method comprises the following steps: accurately weighed amounts of the test materials (examples 1 to 13) and commercially available activated carbon (a: coconut shell granular activated carbon, coconut shell granules 4 to 8mm, specific surface area: 950 m)2(iv)/g, Henan Huansheng carbon industries, Ltd; b: wooden columnar activated carbon, 4mm, specific surface area: 850m2(g, Henan Huanyang carbon industry Co., Ltd.), drying at 80 deg.C, and placing into standard radon chamber (radon initial concentration 10000 Bq/m)3At 25 deg.C and 40% relative humidity) for 48 hr, taking out, sealing, balancing radon and its daughter for 3 hr, measuring with gamma spectrometer (equipped with potassium iodide crystal detector) for 0.5 hr to detect the obtained gammaRay counting is used as an index for measuring radon absorption performance of the material; wherein, after absorbing radon, the commercial coconut shell particle active carbon of unit mass counts 4086 by gamma; and the gamma total count of the unit mass of the commercially available wooden columnar activated carbon after absorbing radon is 79.
Example 1:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
step one, cleaning xanthium fruit shells to remove impurities, drying the xanthium fruit shells in a forced air drying oven at 100 ℃ overnight, heating the xanthium fruit shells under the protection of nitrogen and carbonizing the xanthium fruit shells for 1 hour at 500 ℃, and naturally cooling the xanthium fruit shells to obtain a carbonized material;
step two, fully stirring and mixing the carbonized material and an activating agent KOH according to the weight ratio of 2:1, activating for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling, soaking for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium shell-based biomass carbon material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 3min at intervals after every 10min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 300 kHz;
fig. 1 is an SEM image of the prepared xanthium fruit shell-based biomass charcoal material, and it can be seen from the image that the xanthium fruit shell-based biomass charcoal material has a honeycomb-shaped porous tubular structure with a diameter of 5-10 micrometers, and through the preparation process of the present invention, more nano-pore structures are formed on the honeycomb-shaped microporous wall, so that the xanthium fruit shell-based biomass charcoal material prepared by the present invention has a higher specific surface area.
FIG. 2 shows an XRD pattern of the xanthium fruit shell based biomass charcoal material; it can be seen that characteristic peaks of the xanthium fruit shell-based biomass charcoal material prepared by the method appear near 24 degrees and 43 degrees, and respectively correspond to 002 and 100 graphite crystallite diffraction peaks.
FIG. 5 is a graph showing adsorption and desorption curves of xanthium sibiricum shell-based biomass charcoal material measured by a BET method; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2573.89m2Fig. 6 is a pore size distribution diagram of the xanthium sibiricum shell-based biomass charcoal material; the pore size of the micropores is concentrated and distributed at about 0.5 nm.
The gamma counts before and after radon absorption and after heating regeneration of the prepared xanthium-based biomass charcoal material are shown in figure 3. It can be known that very obvious radon daughter appears after radon inhalation214Pb and214the Bi characteristic peak and the gamma total count 59263 after the unit mass xanthium shell-based biomass charcoal material absorbs radon show that the xanthium shell-based biomass charcoal adsorbent prepared by the method has a very good adsorption effect on radon gas. The characteristic peaks of the radon daughters 214Pb and 214Bi disappear after being heated at the high temperature of 90 ℃, which indicates that radon gas is successfully desorbed and the radon adsorption performance is still close to once after 5 times of adsorption-desorption-regeneration cycles (figure 4);
example 2:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
step one, cleaning xanthium fruit shells to remove impurities, drying the xanthium fruit shells in a forced air drying oven at 100 ℃ overnight, heating the xanthium fruit shells under the protection of nitrogen and carbonizing the xanthium fruit shells for 1 hour at 500 ℃, and naturally cooling the xanthium fruit shells to obtain a carbonized material;
step two, activating agents KOH and K2CO3Mixing the materials according to a weight ratio of 1:1, fully stirring and mixing the materials with a carbonized material according to a weight ratio of 1:1, activating the materials for 2 hours at 850 ℃ under the protection of nitrogen, naturally cooling the materials, soaking the materials in 0.1mol/L diluted hydrochloric acid solution for 5 hours, filtering the materials, washing the materials with deionized water until the filtrate is neutral, and drying the materials to obtain the xanthium shell-based biomass charcoal material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 5min at intervals after every 15min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 350 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2579.24m2And/g, gamma total counting 59987 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 3:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
step one, cleaning xanthium fruit shells to remove impurities, drying the xanthium fruit shells in a forced air drying oven at 100 ℃ overnight, heating the xanthium fruit shells under the protection of nitrogen and carbonizing the xanthium fruit shells for 1 hour at 500 ℃, and naturally cooling the xanthium fruit shells to obtain a carbonized material;
step two, activating agents KOH and K2SiO3Mixing the materials according to a weight ratio of 1:1, fully stirring and mixing the materials with a carbonized material according to a weight ratio of 2:1, activating the materials for 2 hours at 750 ℃ under the protection of nitrogen, naturally cooling the materials, soaking the materials in 0.1mol/L diluted hydrochloric acid solution for 5 hours, filtering the materials, washing the materials with deionized water until the filtrate is neutral, and drying the materials to obtain the xanthium shell-based biomass charcoal material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 5min at intervals after every 10min of ultrasound reaction, wherein the pressure is 22MPa, and the frequency is 300 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2487.15m2And/g, gamma total counting 58997 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 4:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
step one, cleaning xanthium fruit shells to remove impurities, drying the xanthium fruit shells in a forced air drying oven at 100 ℃ overnight, heating the xanthium fruit shells under the protection of nitrogen and carbonizing the xanthium fruit shells for 1 hour at 500 ℃, and naturally cooling the xanthium fruit shells to obtain a carbonized material;
step two, fully stirring and mixing the carbonized material and an activating agent KOH according to the weight ratio of 1:3, activating for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling, soaking for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium shell-based biomass carbon material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 3min at intervals after every 10min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 300 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2513.74m2And/g, gamma total counting 59576 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 5:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
step one, cleaning xanthium fruit shells to remove impurities, drying the xanthium fruit shells in a forced air drying oven at 100 ℃ overnight, heating the xanthium fruit shells under the protection of nitrogen and carbonizing the xanthium fruit shells for 1 hour at 500 ℃, and naturally cooling the xanthium fruit shells to obtain a carbonized material;
step two, mixing the carbonized material and an activating agent K2CO3Fully stirring and mixing the materials according to the weight ratio of 2:1, activating the materials for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling the materials, soaking the materials for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering the materials, washing the materials by using deionized water until the filtrate is neutral, and drying the materials to obtain the xanthium shell-based biomass charcoal material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 5min at intervals after every 12min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 300 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2562.11m2And/g, the gamma total count of the xanthium shell-based biomass charcoal material per unit mass after absorbing radon is 59335.
Example 6:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
cleaning cocklebur fruit shells to remove impurities, drying at 80 ℃, then crushing, uniformly mixing 25g of crushed cocklebur fruit shells, 1g of sodium polyacrylate, 0.8g of polyvinyl alcohol, 1g of sodium bicarbonate and 0.6g of glucosamine to obtain a mixture, then adding the mixture into a ball milling tank of a low-temperature stirring ball mill, adding zirconia grinding balls, and carrying out ball milling by using liquid nitrogen as a ball milling medium to obtain a ball milling material, namely the pretreated cocklebur fruit shells; the liquid nitrogen filling rate in the ball milling tank is 80%, the rotating speed of the stirring ball mill is 300r/min, and the weight ratio of the zirconia grinding balls to the mixture is 8: 1, ball milling for 5 hours; heating the ball-milled material under the protection of nitrogen at 500 ℃ for carbonization for 1 hour, and naturally cooling to obtain a carbonized material;
step two, fully stirring and mixing the carbonized material and an activating agent KOH according to the weight ratio of 2:1, activating for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling, soaking for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium shell-based biomass carbon material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 3min at intervals after every 10min of ultrasound reaction, wherein the total ultrasound time is 2h, the pressure is 20MPa, and the frequency is 300 kHz; the xanthium fruit shell based biomass charcoal materialSpecific surface area of 2754.13m2And/g, gamma total counting 64549 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 7:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
cleaning cocklebur fruit shells to remove impurities, drying at 100 ℃, then crushing, uniformly mixing 30g of crushed cocklebur fruit shells, 2g of sodium polyacrylate, 0.6g of polyvinyl alcohol, 2g of sodium bicarbonate and 0.5g of glucosamine to obtain a mixture, then adding the mixture into a ball milling tank of a low-temperature stirring ball mill, adding zirconia grinding balls, and carrying out ball milling by using liquid nitrogen as a ball milling medium to obtain a ball milling material, namely the pretreated cocklebur fruit shells; the liquid nitrogen filling rate in the ball milling tank is 80%, the rotating speed of the stirring ball mill is 350r/min, and the weight ratio of the zirconia grinding balls to the mixture is 10:1, ball milling for 5 hours; heating the ball-milled material under the protection of nitrogen at 500 ℃ for carbonization for 1 hour, and naturally cooling to obtain a carbonized material;
step two, mixing the carbonized material and an activating agent K2CO3Fully stirring and mixing the materials according to the weight ratio of 2:1, activating the materials for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling the materials, soaking the materials for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering the materials, washing the materials by using deionized water until the filtrate is neutral, and drying the materials to obtain the xanthium shell-based biomass charcoal material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 5min at intervals after every 12min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 300 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2787.87m2And/g, gamma total counting 64789 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 8:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
step one, cleaning xanthium fruit shells to remove impurities, drying the xanthium fruit shells in a forced air drying oven at 100 ℃ overnight, heating the xanthium fruit shells under the protection of nitrogen and carbonizing the xanthium fruit shells for 1 hour at 500 ℃, and naturally cooling the xanthium fruit shells to obtain a carbonized material;
step two, weighingThe ratio of 2:1 is carbonized material and activating agent K2CO3Adding into a hydrothermal reaction kettle, adding deionized water, sealing the hydrothermal reaction kettle, heating and reacting at 370 ℃ and 22MPa for 60min, cooling, and filtering; the weight ratio of the carbonized material to the deionized water is 1: 40; drying the filtered carbonized material, activating for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling, soaking for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium shell-based biomass carbon material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 5min at intervals after every 12min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 300 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2695.98m2And/g, gamma total counting 63358 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 9:
a preparation method of a xanthium sibiricum shell-based biomass charcoal material comprises the following steps:
cleaning cocklebur fruit shells to remove impurities, drying at 100 ℃, then crushing, uniformly mixing 30g of crushed cocklebur fruit shells, 2g of sodium polyacrylate, 0.6g of polyvinyl alcohol, 2g of sodium bicarbonate and 0.5g of glucosamine to obtain a mixture, then adding the mixture into a ball milling tank of a low-temperature stirring ball mill, adding zirconia grinding balls, and carrying out ball milling by using liquid nitrogen as a ball milling medium to obtain a ball milling material, namely the pretreated cocklebur fruit shells; the liquid nitrogen filling rate in the ball milling tank is 80%, the rotating speed of the stirring ball mill is 350r/min, and the weight ratio of the zirconia grinding balls to the mixture is 10:1, ball milling for 5 hours; heating the ball-milled material under the protection of nitrogen at 500 ℃ for carbonization for 1 hour, and naturally cooling to obtain a carbonized material;
step two, taking the carbonized material and an activating agent K in a weight ratio of 2:12CO3Adding into a hydrothermal reaction kettle, adding deionized water, sealing the hydrothermal reaction kettle, heating and reacting at 370 ℃ and 22MPa for 60min, cooling, and filtering; the weight ratio of the carbonized material to the deionized water is 1: 40; drying the filtered carbonized material, drying the carbonized material,then activating for 2 hours at 800 ℃ under the protection of nitrogen, naturally cooling, soaking for 5 hours by using 0.1mol/L diluted hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium fruit shell-based biomass charcoal material; in the process of soaking by using dilute hydrochloric acid solution, sealed pressurized ultrasound is adopted, and the technological parameters are as follows: stopping ultrasound for 5min at intervals after every 12min of ultrasound reaction, wherein the pressure is 20MPa, and the frequency is 300 kHz; the specific surface area of the xanthium fruit shell-based biomass charcoal material is 2895.68m2And/g, gamma total counting 68984 after the xanthium shell-based biomass charcoal material absorbs radon in unit mass.
Example 10:
a method for preparing a cocklebur fruit shell based biomass charcoal adsorbent by using the cocklebur fruit shell based biomass charcoal material of example 1, comprising the following steps:
step A, adding 120g of xanthium-based biomass charcoal material into a mixer, then adding 2g of oleic acid and 25g of plasticizing binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2 days;
step B, adding the aged and decayed mixture into a vacuum pugging machine for vacuum pugging for 3 times, wherein each time lasts for 45 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; putting the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60 ℃; the pressure of extrusion forming is 15 MPa;
d, calcining the dried product at 650 ℃ for 3 hours; then heating to 850 ℃, introducing carbon dioxide, activating for 5 hours, and naturally cooling to obtain the xanthium sibiricum-based biomass charcoal adsorbent; introducing carbon dioxide at a speed of 200 sccm;
the preparation method of the plasticized binder comprises the following steps: adding 3g of water-soluble starch, 4g of trehalose, 1.5g of mannitol, 0.8g of polyvinylpyrrolidone and 0.4g of polyethyleneimine into 23g of water, and stirring at 300r/min for 30min to obtain a plasticized binder;
gamma total count 58688 after radon absorption by unit mass xanthium biomass charcoal adsorbent.
Example 11:
a method for preparing a cocklebur fruit shell based biomass charcoal adsorbent using the cocklebur fruit shell based biomass charcoal material of example 6, comprising the steps of:
step A, adding 100g of xanthium-based biomass charcoal material into a mixer, then adding 3g of oleic acid and 35g of plasticized binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2 days;
step B, adding the aged and decayed mixture into a vacuum pugging machine for vacuum pugging for 3 times, wherein each time lasts for 45 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; putting the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60 ℃; the pressure of extrusion forming is 18 MPa;
d, calcining the dried product at 700 ℃ for 3 hours; then heating to 900 ℃, introducing carbon dioxide, activating for 5 hours, and naturally cooling to obtain the xanthium sibiricum-based biomass charcoal adsorbent; introducing carbon dioxide at a speed of 200 sccm;
the preparation method of the plasticized binder comprises the following steps: 5g of water-soluble starch, 2g of trehalose, 2g of mannitol, 0.8g of polyvinylpyrrolidone and 0.4g of polyethyleneimine are added into 22g of water, and stirred for 30min at 300r/min to obtain the plasticized binder.
And (3) gamma total counting 64014 after absorbing radon by using the xanthium biomass charcoal adsorbent with unit mass.
Example 12:
a method for preparing a cocklebur fruit shell based biomass charcoal adsorbent using the cocklebur fruit shell based biomass charcoal material of example 7, comprising the steps of:
step A, adding 100g of xanthium-based biomass charcoal material into a mixer, then adding 3g of oleic acid and 35g of plasticized binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2 days;
step B, adding the aged and decayed mixture into a vacuum pugging machine for vacuum pugging for 3 times, wherein each time lasts for 45 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; putting the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60 ℃; the pressure of extrusion forming is 18 MPa;
d, calcining the dried product at 700 ℃ for 3 hours; then heating to 900 ℃, introducing carbon dioxide, activating for 5 hours, and naturally cooling to obtain the xanthium sibiricum-based biomass charcoal adsorbent; introducing carbon dioxide at a speed of 200 sccm;
the preparation method of the plasticized binder comprises the following steps: 5g of water-soluble starch, 2g of trehalose, 2g of mannitol, 0.8g of polyvinylpyrrolidone and 0.4g of polyethyleneimine are added into 22g of water, and stirred for 30min at 300r/min to obtain the plasticized binder.
Gamma total count 64089 after radon absorption by unit mass xanthium biomass charcoal adsorbent.
Example 13:
a method for preparing a cocklebur fruit shell based biomass charcoal adsorbent using the cocklebur fruit shell based biomass charcoal material of example 8, comprising the steps of:
step A, adding 100g of xanthium-based biomass charcoal material into a mixer, then adding 3g of oleic acid and 35g of plasticized binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2 days;
step B, adding the aged and decayed mixture into a vacuum pugging machine for vacuum pugging for 3 times, wherein each time lasts for 45 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; putting the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60 ℃; the pressure of extrusion forming is 18 MPa;
d, calcining the dried product at 700 ℃ for 3 hours; then heating to 900 ℃, introducing carbon dioxide, activating for 5 hours, and naturally cooling to obtain the xanthium sibiricum-based biomass charcoal adsorbent; introducing carbon dioxide at a speed of 200 sccm;
the preparation method of the plasticized binder comprises the following steps: 5g of water-soluble starch, 2g of trehalose, 2g of mannitol, 0.8g of polyvinylpyrrolidone and 0.4g of polyethyleneimine are added into 22g of water, and stirred for 30min at 300r/min to obtain the plasticized binder.
Gamma total count 63007 after radon absorption by unit mass xanthium biomass charcoal adsorbent.
Example 14:
a method for preparing a cocklebur fruit shell based biomass charcoal adsorbent using the cocklebur fruit shell based biomass charcoal material of example 9, comprising the steps of:
step A, adding 100g of xanthium-based biomass charcoal material into a mixer, then adding 3g of oleic acid and 35g of plasticized binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2 days;
step B, adding the aged and decayed mixture into a vacuum pugging machine for vacuum pugging for 3 times, wherein each time lasts for 45 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; putting the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60 ℃; the pressure of extrusion forming is 18 MPa;
d, calcining the dried product at 700 ℃ for 3 hours; then heating to 900 ℃, introducing carbon dioxide, activating for 5 hours, and naturally cooling to obtain the xanthium sibiricum-based biomass charcoal adsorbent; introducing carbon dioxide at a speed of 200 sccm;
the preparation method of the plasticized binder comprises the following steps: 5g of water-soluble starch, 2g of trehalose, 2g of mannitol, 0.8g of polyvinylpyrrolidone and 0.4g of polyethyleneimine are added into 22g of water, and stirred for 30min at 300r/min to obtain the plasticized binder.
Gamma total count 68112 after radon absorption by xanthium biomass charcoal adsorbent per unit mass.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.

Claims (9)

1. The preparation method of the xanthium sibiricum shell-based biomass charcoal material is characterized by comprising the following steps:
cleaning cocklebur fruit shells to remove impurities, heating at 450-550 ℃ under the protection of inert gas for carbonization for 0.5-1.5 hours, and naturally cooling to obtain a carbonized material;
step two, fully mixing the carbonized material and an activating agent according to a weight ratio of 1-10: 1-3, activating for 1-3 hours at 600-800 ℃ under the protection of inert gas, naturally cooling, soaking for 4-6 hours by using a dilute hydrochloric acid solution, filtering, washing by using deionized water until the filtrate is neutral, and drying to obtain the xanthium shell-based biomass carbon material;
the cocklebur fruit shell-based biomass charcoal material prepared by the preparation method is applied to adsorption of radioactive radon gas in an atmospheric environment, radioactive radon gas in a underground closed space of a uranium tailing area, radioactive radon gas in a household house and radioactive radon gas in an office place.
2. The method for preparing the xanthium fruit shell-based biomass charcoal material as claimed in claim 1, wherein the inert gas is nitrogen, and the activating agent is KOH or K2CO3And K2SiO3One or any combination of two or more of them.
3. The preparation method of the xanthium fruit shell-based biomass charcoal material as claimed in claim 1, wherein the concentration of the dilute hydrochloric acid solution is 0.08-0.12 mol/L.
4. The preparation method of the xanthium fruit shell-based biomass charcoal material as claimed in claim 1, wherein in the first step, the following pretreatment is further performed on the xanthium fruit shell before carbonization: drying the cleaned cocklebur fruit shells at 80-100 ℃, then crushing, uniformly mixing 20-30 parts of crushed cocklebur fruit shells, 1-2 parts of sodium polyacrylate, 0.5-0.8 part of polyvinyl alcohol, 1-2 parts of sodium bicarbonate and 0.5-0.8 part of glucosamine according to parts by weight to obtain a mixture, then adding the mixture into a ball milling tank of a low-temperature stirring ball mill, adding zirconia milling balls, and carrying out ball milling by using liquid nitrogen as a ball milling medium to obtain ball milling materials, namely the pretreated cocklebur fruit shells; the liquid nitrogen filling rate in the ball milling tank is 80-85%, the rotating speed of the stirring ball mill is 300-450 r/min, and the weight ratio of the zirconia grinding balls to the mixture is 8-10: 1, the ball milling time is 5-6 h.
5. The preparation method of the xanthium sibiricum shell-based biomass charcoal material according to claim 1, wherein in the second step, the process of fully mixing the charring material and the activating agent according to the weight ratio of 1-10: 1-3 comprises the following steps: adding a carbonized material and an activating agent into a hydrothermal reaction kettle, adding deionized water, sealing the hydrothermal reaction kettle, heating and reacting at 365-375 ℃ and under 20-24 MPa for 45-60 min, cooling, and filtering, wherein the weight ratio of the carbonized material to the deionized water is 1: 30-50.
6. The preparation method of the xanthium fruit shell-based biomass charcoal material as claimed in claim 1, wherein in the second step, sealed pressurized ultrasound is adopted in the process of soaking with dilute hydrochloric acid solution, and the process parameters are as follows: stopping ultrasound for 3-5 min at intervals after every 10-15 min of ultrasound reaction, wherein the pressure is 15-22 MPa, and the frequency is 300-450 kHz.
7. A method for preparing the cocklebur fruit shell based biomass charcoal adsorbent by using the cocklebur fruit shell based biomass charcoal material according to any one of claims 1 to 6, which is characterized by comprising the following steps:
step A, adding 80-120 parts by weight of xanthium fruit shell-based biomass charcoal material into a pugmill, then adding 2-4 parts by weight of oleic acid and 25-35 parts by weight of plasticizing binding agent while stirring until the materials are uniformly mixed to obtain a mixture, and placing the mixture in a sealed container for ageing for 2-3 days;
b, adding the aged mixture into a vacuum pugging machine for vacuum pugging for 3-4 times, wherein each time lasts for 45-60 min;
step C, cutting the mixture subjected to vacuum pugging into blanks; placing the blank section into a ceramic tube extruding machine with a honeycomb die, carrying out extrusion forming, and then drying at 60-80 ℃; the pressure for extrusion molding is 10-20 MPa;
d, calcining the dried product at 600-800 ℃ for 2-3 hours; then heating to 850-900 ℃, introducing carbon dioxide, activating for 3-5 hours, and naturally cooling to obtain the xanthium fruit shell-based biomass carbon adsorbent; the carbon dioxide was introduced at a rate of 200 sccm.
8. The method for preparing the cocklebur fruit shell based biomass charcoal adsorbent by using the cocklebur fruit shell based biomass charcoal material according to claim 7, wherein the preparation method of the plasticized binder is as follows: according to parts by weight, 1-5 parts of water-soluble starch, 2-6 parts of trehalose, 1-2 parts of mannitol, 0.5-0.8 part of polyvinylpyrrolidone and 0.3-0.5 part of polyethyleneimine are added into 20-23 parts of water, and the mixture is stirred for 30-45 min at the speed of 100-300 r/min to obtain the plasticized binder.
9. The application of the cocklebur fruit shell based biomass charcoal adsorbent prepared according to the preparation method of claim 7 in adsorption of radioactive radon gas in atmospheric environment, radioactive radon gas in underground closed space of uranium tailing area, radioactive radon gas in household residence and radioactive radon gas in office.
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