CN106631153B - Method for loading easily sublimable substance in aerogel material - Google Patents

Method for loading easily sublimable substance in aerogel material Download PDF

Info

Publication number
CN106631153B
CN106631153B CN201611241817.3A CN201611241817A CN106631153B CN 106631153 B CN106631153 B CN 106631153B CN 201611241817 A CN201611241817 A CN 201611241817A CN 106631153 B CN106631153 B CN 106631153B
Authority
CN
China
Prior art keywords
aerogel material
piston
substance
cylinder
aerogel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201611241817.3A
Other languages
Chinese (zh)
Other versions
CN106631153A (en
Inventor
燕映霖
陈利萍
王岩
杨蓉
许云华
任冰
李巧乐
秦海超
史忙忙
魏一奇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian University of Technology
Original Assignee
Xian University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian University of Technology filed Critical Xian University of Technology
Priority to CN201611241817.3A priority Critical patent/CN106631153B/en
Publication of CN106631153A publication Critical patent/CN106631153A/en
Application granted granted Critical
Publication of CN106631153B publication Critical patent/CN106631153B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5093—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with elements other than metals or carbon
    • C04B41/5097—Sulfur
    • 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
    • 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
    • B01D53/002—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 condensation
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5007—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing
    • C04B41/5011—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing containing halogen in the anion
    • C04B41/5012—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing containing halogen in the anion chlorides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5093—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with elements other than metals or carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/202—Single element halogens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/206—Organic halogen compounds
    • B01D2257/2064—Chlorine
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • B01D2257/7027—Aromatic hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/708—Volatile organic compounds V.O.C.'s

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)

Abstract

A method for loading easily sublimable substance in aerogel material comprises placing easily sublimable substance into the bottom of a piston-sealed cylinder, stacking aerogel material on the upper part, and placing into a piston; exhausting air in the cylinder and the aerogel material, and introducing inert gas through an outlet of the cylinder; sealing the outlet of the cylinder, quickly pushing and pressing the piston, and heating inert gas in the cylinder due to sudden compression so that the easily sublimed substance is heated and sublimated and enters the pore channel of the aerogel material under the pressure of the piston; rapidly drawing the piston to the initial length of the aerogel material, wherein the temperature of the inert gas is reduced due to volume expansion, and along with the reduction of the temperature, the gas-phase easily-raised substances are condensed to form nano-scale particles which are uniformly dispersed in the pore channels of the aerogel material; aerogel materials with high loading of easily-lifting substances are obtained. The method has high load and uniform distribution of the easily sublimable substances, and can be used for treating industrial waste gas containing the easily sublimable substances and preparing uniform composite materials.

Description

Method for loading easily sublimable substance in aerogel material
Technical Field
The invention belongs to the field of environmental protection or composite materials, and particularly relates to a method for loading a sublimable substance in an aerogel material.
Background
With the advance of the human industrialization process, earth resources are increasingly exhausted, and people pay more attention to the recycling of the existing energy sources while being urgent to find novel energy sources. In addition, environmental pollution caused by the use of fossil fuel is also a problem suffered by environmental protection people and scientists. Since the eighties of the last century, the problems of resource exhaustion and environmental pollution are increasingly highlighted while national economy is rapidly developed in China. As a big coal country in China, coal resources account for more than half of the total resource reserves, and the coal resources are often accompanied by huge wastes in mining, processing and power generation applications, and the generated industrial three wastes (waste residues, waste water and wastes) are the key problems of green reform and recyclable development of the industry in China.
Aerogel materials, also known as xerogels. When most of the solvent is removed from the gel, the liquid content in the gel is much less than the solid content, or the space network structure of the gel is filled with gas, and the appearance is solid, namely xerogel, also called aerogel. Aerogel is a solid form, one of the world's less dense solids. The density was 3 kg per cubic meter. A common aerogel is a silica aerogel, which was first produced by Kistler, the american scientist, in 1931 because of gambling with her friends. There are many kinds of aerogels, including silicon-based, carbon-based, sulfur-based, metal oxide-based, metal-based, and the like. Aerogel materials have important research values in the fractal structure research field, the thermal insulation material research field and the sound insulation material research field.
In recent years, in the field of energy storage materials, carbon aerogel as a novel conductive porous material is a novel carbon material developed after fibrous activated carbon, and has a large specific surface area (600- & ltSUB & gt 1000 m- & gt)2/kg) and high conductivity (10-25 s/cm). Moreover, the density variation range is wide (0.05-1.0 g/cm)3). If the micro-hole is filled with proper electrolyte, a novel rechargeable battery can be made, which has the excellent characteristics of large storage capacity, small internal resistance, light weight, strong charge-discharge capacity, repeated use and the like, and the preliminary experiment result shows that: the charge capacity of the carbon aerogel reaches 3 x 104/kg2The power density is 7kw/kg, the repeated charge-discharge performance is good, and the catalyst is widely applied to various fields such as electrochemistry, catalysis and environmental protection.
The existing method for loading simple substance easily-lifting substance on aerogel mainly comprises the following steps:
(1) an adsorption method: the aerogel material is pressed and packaged to form an adsorption bag or an adsorption module, and the high surface adsorption capacity of the adsorption bag or the adsorption module is utilized to adsorb the easily-liftable substance elements in the passing waste gas containing the easily-liftable substance. Although the method has simple process, the aerogel with high specific surface area and pore volume cannot be fully utilized, the aerogel is easy to be poisoned, and the efficiency of loading easily-raised substances is low.
(2) Solvent exchange method: dissolving the easily sublimable substance into organic solvents of ethanol, ether, carbon disulfide, carbon tetrachloride, propane, butane, pentane, hexane, cyclohexane, toluene and benzene, soaking the solvents into the aerogel material, evaporating the organic solvents, and precipitating the easily sublimable substance out again and loading the easily sublimable substance in the aerogel material. However, in the method, the organic solvent is difficult to enter a microporous structure, so that the negative easily-lifting substance is insufficient and not uniform, the organic solvent is toxic, and the organic solvent needs to be refluxed and condensed for recycling after evaporation, so that the process is complex, and the cost is difficult to reduce.
(3) The chemical method comprises the following steps: dissolving a reaction raw material of a readily liftable substance in a solvent, dispersing an aerogel material in the solvent, and exciting a reaction under a certain condition to generate simple substance readily liftable substance particles loaded in the aerogel material. However, in the method, the organic solvent is difficult to enter the microporous structure, so that the easily-sublimed substance is insufficiently and unevenly loaded, chemical reaction is required to be carried out under controlled conditions, the reaction precision is difficult to control, the process is complex, and the cost is high.
(4) A heat treatment method: mixing the simple substance easily-lifting substance and the aerogel material according to a certain proportion, sealing the mixture in a special container after stirring and ball milling, vacuumizing or introducing inert atmosphere for protection, then sending the mixture into a heat treatment furnace for treatment at 40-150 ℃ for 1-8 hours, heating the mixture to more than 300 ℃ for treatment for 1-3 hours, removing the redundant simple substance easily-lifting substance which is not well compounded, and cooling the mixture to room temperature along with the furnace to complete the process of loading the simple substance easily-lifting substance by the aerogel. The method has the disadvantages of harsh process conditions, long loading time and difficulty in realizing an automatic process.
Disclosure of Invention
The invention aims to provide a method for loading easily sublimable substances in an aerogel material, which has the advantages of high quality of the easily sublimable substances, uniform distribution of simple substances of the easily sublimable substances, environmental protection and greenness.
The technical scheme adopted by the invention is that the method for loading the easily sublimable substance in the aerogel material is implemented according to the following steps:
step 1, placing a simple substance easy to sublimate into the bottom of a piston sealing cylinder, stacking an aerogel material on the upper part of the simple substance easy to sublimate, and placing the aerogel material into a piston;
step 2, exhausting air in the cylinder and the aerogel material, and then introducing inert gas through an outlet of the cylinder;
step 3, sealing the outlet of the cylinder, quickly pushing and pressing the piston, and heating inert gas in the cylinder due to sudden compression so that the easy-to-rise substance simple substance is heated and sublimated and enters the pore channel of the aerogel material under the pressure of the piston;
step 4, rapidly drawing the piston to the initial length of the aerogel material, wherein the temperature of the inert gas is reduced due to volume expansion, and along with the reduction of the temperature, the gas-phase easily-raised substances are condensed to form nano-scale particles which are uniformly dispersed in the pore channel of the aerogel material;
and 5, repeating the 2-4 steps to obtain the aerogel material with high loading capacity of the easily-lifting substances.
The present invention is also characterized in that,
in the step 1, the mass ratio of the aerogel material to the simple substance easy-to-sublimate substance is 1: 4-5.
The aerogel material is a carbon aerogel material or a silicon aerogel material.
The simple substance easy-sublimation substance is one or a mixture of more of sulfur, iodine, naphthalene or aluminum trichloride.
In the step 2, the inert gas is one or a mixture of more of nitrogen, helium, neon, argon or xenon.
In the step 3, the compression ratio of the inert gas in the cylinder is 2-10.
The pushing speed of the piston in the step 3 is 0.2-1 m/s.
The method for loading the easily sublimable substance in the aerogel material has the following characteristics:
(1) green and environment-friendly: according to the invention, the simple substance easily-sublimed substance is gasified and then condensed in the aerogel material to realize the loading of the easily-sublimed substance, so that no heat source is required for heating, and no waste is generated;
(2) the easily-lifting substance is efficiently and uniformly loaded: the air in the aerogel material is discharged before loading, so that the gas-phase easily-lifting substance can enter the multilevel pore channel structure of the aerogel, the structural advantages of the aerogel material are fully exerted, and on the other hand, the gas-phase easily-lifting substance is high in cooling speed and fine in particle size after solidification, so that the uniformity degree of the aerogel loading easily-lifting substance is optimized;
(3) the process is simple and controllable: the loading method is simple, the loading capacity of the aerogel material can be adjusted by controlling the push-pull times, in addition, the method is easy to expand and automate, and if the continuous easily-upgraded substance source and the continuously-replaced aerogel material can be provided, the automatic continuous batch production can be realized.
In conclusion, the invention provides a method for loading simple substance easily-lifting substances on an aerogel material, which is simple, convenient and easy to operate and easy to automate, and the obtained easily-lifting substance/aerogel composite material has the characteristics of high loading amount and uniform distribution.
Drawings
FIG. 1 is a process schematic of the process of the present invention;
FIG. 2 is a scanning electron micrograph of the carbon gel material used in example 1;
FIG. 3 is a thermogravimetric plot of the elemental sulfur/carbon aerogel composite prepared as in example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The method for loading the easily sublimable substance in the aerogel material has the specific process shown in figure 1, and is implemented according to the following steps:
step 1, placing a simple substance easy to sublimate into the bottom of a piston sealing cylinder, stacking an aerogel material on the upper part of the simple substance easy to sublimate, and placing the aerogel material into a piston; the mass ratio of the aerogel material to the simple substance easy-to-sublimate substance is 1: 4-5; the aerogel material is a carbon aerogel material or a silicon aerogel material; the simple substance easy-sublimation substance is one or a mixture of more of sulfur, iodine, naphthalene or aluminum trichloride;
step 2, discharging air in the cylinder and in the aerogel material, and then introducing inert gas (the inert gas is one or a mixture of nitrogen, helium, neon, argon or xenon) through an outlet of the cylinder until the compression ratio of the inert gas in the cylinder is 2-10;
step 3, sealing the outlet of the cylinder, quickly pushing the piston at a pushing speed of 0.2-1m/s, and heating inert gas in the cylinder due to sudden compression so that the easily sublimable substance is heated and sublimated and enters the pore channel of the aerogel material under the pressure of the piston;
step 4, rapidly drawing the piston to the initial length of the aerogel material, wherein the temperature of the inert gas is reduced due to volume expansion, and along with the reduction of the temperature, the gas-phase easily-raised substances are condensed to form nano-scale particles which are uniformly dispersed in the pore channel of the aerogel material;
and 5, repeating the 2-4 steps to obtain the aerogel material with high loading capacity of the easily-lifting substances.
Example 1
(1) Vessel conduits used for pretreatment: cleaning the used cylinder and piston with deionized water, and drying in a forced air drying oven at 80 deg.C for 10 hr to remove surface water;
(2) putting 5g of sublimed sulfur into the bottom of a piston sealing cylinder, stacking 1g of carbon aerogel material on the piston sealing cylinder, and filling the piston with the carbon aerogel material;
(3) pushing and pressing the piston to drive the bottom of the cylinder, completely discharging air in the cylinder and in the carbon aerogel, connecting the outlet of the cylinder with nitrogen, and drawing the piston to charge the nitrogen until the compression ratio is 2;
(4) sealing an outlet of the cylinder, quickly pushing and pressing the piston at the pushing and pressing speed of 0.2m/s, heating nitrogen in the cylinder due to sudden compression, heating sublimed sulfur, and enabling the sublimed sulfur to enter a pore channel of the carbon aerogel material under the pressure of the piston;
(5) rapidly drawing the piston to the initial length of the carbon aerogel material, wherein the temperature of the nitrogen is reduced due to volume expansion, and the gaseous sublimed sulfur is condensed to form nano-scale particles which are uniformly dispersed in the pore channel of the carbon aerogel material;
(6) and pulling out the piston, and taking out the composite material, namely obtaining the sulfur/carbon aerogel composite material with high load.
Fig. 2 is a scanning electron micrograph of the carbon aerogel used in example 1, and it can be seen from fig. 2 that the carbon aerogel has a three-dimensional self-assembled structure and a large number of multi-level pore structures, and can effectively adsorb volatile substances.
Fig. 3 is a thermogravimetric plot of the sulfur/carbon aerogel composite and the carbon aerogel material obtained in example 1, and it can be seen from the comparison in fig. 3 that the sulfur loading of the prepared sulfur/carbon aerogel composite reaches 75%.
Example 2
(1) Vessel conduits used for pretreatment: cleaning the used cylinder and piston with deionized water, and drying in a forced air drying oven at 100 deg.C for 24 hr to remove surface water;
(2) 20g of elemental iodine is placed at the bottom of a piston sealing cylinder, 5g of silicon aerogel material is stacked on the elemental iodine, and the elemental iodine is placed into a piston;
(3) pushing and pressing the piston to drive the bottom of the cylinder, completely discharging air in the cylinder and in the silicon aerogel, connecting the outlet of the cylinder with argon, and drawing the piston to charge the argon until the compression ratio is 10;
(4) sealing the outlet of the cylinder, quickly pushing and pressing the piston at the pushing and pressing speed of 1m/s, heating the argon in the cylinder due to sudden compression, heating and sublimating the elemental iodine, and enabling the elemental iodine to enter a pore channel of the silicon aerogel material under the pressure of the piston;
(5) rapidly drawing the piston to the initial length of the aerogel material, wherein the temperature of the argon gas is reduced due to volume expansion, and gaseous elementary iodine is condensed to form nano-scale particles which are uniformly dispersed in the pore channel of the silicon aerogel material;
(6) and (5) repeating the operation of the step (3-5) for five times, pulling out the piston, and taking out the composite material to obtain the iodine/silicon aerogel composite material with high load.
Example 3
(1) Vessel conduits used for pretreatment: cleaning the used cylinder and piston with deionized water, and drying in a forced air drying oven at 90 deg.C for 16h to remove surface water;
(2) 10g of elemental naphthalene is placed at the bottom of a piston sealing cylinder, 2g of carbon aerogel material is stacked on the elemental naphthalene, and the carbon aerogel material is placed into a piston;
(3) pushing and pressing the piston to drive the bottom of the cylinder, completely discharging air in the cylinder and in the carbon aerogel, connecting the outlet of the cylinder with nitrogen and argon mixed gas, and drawing the piston to fill the nitrogen and argon mixed gas until the compression ratio is 6;
(4) sealing the outlet of the cylinder, quickly pushing the piston at the pushing speed of 0.6m/s, and heating the nitrogen-argon mixed gas in the cylinder due to sudden compression, so that the elemental naphthalene is heated and sublimated and enters a pore channel of the carbon aerogel material under the pressure of the piston;
(5) rapidly drawing the piston to the initial length of the aerogel material, wherein the temperature of the nitrogen-argon mixed gas is reduced due to volume expansion, and the gaseous simple substance naphthalene is condensed to form nano-scale particles which are uniformly dispersed in the pore channel of the carbon aerogel material;
(6) repeating the step (3-5) for three times, pulling out the piston, and taking out the composite material to obtain the high-load naphthalene/carbon aerogel composite material.

Claims (3)

1. A method for loading a sublimable substance in an aerogel material is characterized by comprising the following steps:
step 1, placing a simple substance easy to sublimate into the bottom of a piston sealing cylinder, stacking an aerogel material on the upper part of the simple substance easy to sublimate, and placing the aerogel material into a piston; the mass ratio of the aerogel material to the simple substance easy-to-sublimate substance is 1: 4-5; the aerogel material is a carbon aerogel material or a silicon aerogel material; the simple substance easy-sublimation substance is one or a mixture of more of sulfur, iodine, naphthalene or aluminum trichloride;
step 2, exhausting air in the cylinder and the aerogel material, and then introducing inert gas through an outlet of the cylinder;
step 3, sealing the outlet of the cylinder, quickly pushing and pressing the piston, and heating inert gas in the cylinder due to sudden compression so that the simple substance of the easily sublimed substance is heated and sublimated and enters the pore channel of the aerogel material under the pressure of the piston; the pushing speed of the piston is 0.2-1 m/s;
step 4, rapidly drawing the piston to the initial length of the aerogel material, wherein the temperature of the inert gas is reduced due to volume expansion, and along with the reduction of the temperature, the gas-phase easily-sublimed substance is condensed to form nano-scale particles which are uniformly dispersed in the pore channel of the aerogel material;
and 5, repeating the 2-4 steps to obtain the aerogel material with high load of the easily sublimed substance.
2. The method of claim 1, wherein the inert gas in step 2 is one or more of helium, neon, argon, or xenon.
3. The method for supporting a sublimable substance in an aerogel material as claimed in claim 1 or 2, wherein the inert gas compression ratio in the cylinder in the step 3 is 2-10.
CN201611241817.3A 2016-12-29 2016-12-29 Method for loading easily sublimable substance in aerogel material Active CN106631153B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611241817.3A CN106631153B (en) 2016-12-29 2016-12-29 Method for loading easily sublimable substance in aerogel material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611241817.3A CN106631153B (en) 2016-12-29 2016-12-29 Method for loading easily sublimable substance in aerogel material

Publications (2)

Publication Number Publication Date
CN106631153A CN106631153A (en) 2017-05-10
CN106631153B true CN106631153B (en) 2020-02-18

Family

ID=58835409

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611241817.3A Active CN106631153B (en) 2016-12-29 2016-12-29 Method for loading easily sublimable substance in aerogel material

Country Status (1)

Country Link
CN (1) CN106631153B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107204449A (en) * 2017-06-25 2017-09-26 苏州思创源博电子科技有限公司 A kind of preparation method of carbon gel lithium sulfur battery anode material
CN107275613A (en) * 2017-06-25 2017-10-20 苏州思创源博电子科技有限公司 A kind of preparation method of carbon gel composite lithium manganate material
CN107331846A (en) * 2017-07-11 2017-11-07 苏州思创源博电子科技有限公司 A kind of preparation method of sodium-ion battery composite positive pole
CN107302085A (en) * 2017-07-14 2017-10-27 苏州思创源博电子科技有限公司 A kind of carbon gel loads the preparation method of sodium ion battery electrode material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101562244A (en) * 2009-06-02 2009-10-21 北京理工大学 Method for preparing elemental sulfur composite material used by lithium secondary battery
CN105304908A (en) * 2015-10-16 2016-02-03 广东烛光新能源科技有限公司 Preparation method of sulfur-containing electrode material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101562244A (en) * 2009-06-02 2009-10-21 北京理工大学 Method for preparing elemental sulfur composite material used by lithium secondary battery
CN105304908A (en) * 2015-10-16 2016-02-03 广东烛光新能源科技有限公司 Preparation method of sulfur-containing electrode material

Also Published As

Publication number Publication date
CN106631153A (en) 2017-05-10

Similar Documents

Publication Publication Date Title
CN106631153B (en) Method for loading easily sublimable substance in aerogel material
CN106145096B (en) Three-dimensional graphene production method and device, composite electrode material, preparation and application
CN109037662B (en) Preparation method of sulfur-carbon composite positive electrode material for lithium-sulfur battery
CN105826527B (en) A kind of porous silicon-carbon composite and its preparation method and application
CN102148368A (en) Preparation method of lithium ion battery anode composite material and special device thereof
CN101817520B (en) Method for manufacturing carbon microspheres by using waste macromolecules
CN109755482A (en) Silicon/carbon composite and preparation method thereof
CN108439369B (en) Nitrogen-oxygen co-doped hollow carbon nano-microsphere as well as preparation method and application thereof
CN106887567A (en) A kind of carbon coating silicon/graphene composite material and preparation method thereof
CN112713274A (en) Nano silicon-carbon composite material, preparation method, application and lithium ion battery
CN112186162A (en) High-load high-surface-capacity lithium-sulfur battery positive electrode and preparation method and application thereof
CN112635202A (en) Nickel cobaltate @ graphene @ China fir composite material electrode and preparation method and application thereof
CN115172711A (en) Black phosphorus-carbon composite material and preparation method and application thereof
Wang et al. ZIF-67-derived porous nitrogen-doped carbon shell encapsulates photovoltaic silicon cutting waste as anode in high-performance lithium-ion batteries
CN108598417B (en) Conductive carbon black modified silica aerogel sulfur-loaded composite cathode material and preparation method thereof
CN112563042B (en) Biomass carbon aerogel-MnOxPreparation method and application of composite electrode material
Liu et al. Self-swelling derived frameworks with rigidity and flexibility enabling high-reversible silicon anodes
CN117727897A (en) Graphene/carbon nano tube/ferrosilicon alloy-silicon composite anode material and preparation method thereof
CN109012664A (en) A kind of amorphous carbon supported nano-gold metal particles catalyst and its preparation method and application
CN110504450B (en) Preparation method of heteroatom-doped hierarchical pore carbon material and application of heteroatom-doped hierarchical pore carbon material in lithium battery negative electrode slurry
CN112408317A (en) Carbon-loaded titanium dioxide-doped lithium aluminum hydride hydrogen storage material and preparation method thereof
CN104201009B (en) A kind of preparation method of the polymer with nitrogen for electrode material for super capacitor
CN110255537A (en) A kind of preparation method of the three-dimensional porous graphene of high-ratio surface boron atom doping
CN116101974A (en) Aluminum hydride hydrogen storage material doped with polymer and preparation method thereof
CN114094081B (en) Crosslinked nano carbon sheet loaded boron nitride nanocrystalline/sulfur composite material, preparation method thereof, lithium sulfur battery positive electrode and lithium sulfur battery

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant