CN106637090B - A method of loading easy sublimate in the porous material - Google Patents
A method of loading easy sublimate in the porous material Download PDFInfo
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- CN106637090B CN106637090B CN201611241812.0A CN201611241812A CN106637090B CN 106637090 B CN106637090 B CN 106637090B CN 201611241812 A CN201611241812 A CN 201611241812A CN 106637090 B CN106637090 B CN 106637090B
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- porous material
- easy sublimate
- sealing container
- sublimate
- easy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0694—Halides
Abstract
The invention discloses the methods that one kind loads easy sublimate in the porous material, and the easy sublimate of simple substance is added in sealing container, pretreated porous material is loaded in cooling device；It is passed through inert atmosphere into sealing container, and opens vacuum pump, makes to keep negative pressure in sealing container, until excluding the air in evaporation-cooled device completely；Sealing container is heated, makes the easy sublimate of simple substance by the easy sublimate steam of heat sublimation, and be gradually filled with cooling device；Cooling device is opened, load certain time is kept according to porous material quality, obtains the composite material that load capacity is high, is evenly distributed.The present invention realizes the easy sublimate of load by will condense after the easy sublimate gasification of simple substance in porous material surface, reaction temperature is low, no waste generates, improve the load capacity of porous material, since the easy sublimate cooling velocity of gas phase is fast, grain diameter is tiny after solidification, optimizes the uniformity coefficient of the easy sublimate of porous material loading.
Description
Technical field
The invention belongs to environmental protection or new energy fields, and in particular to one kind loads the side of easy sublimate in the porous material
Method.
Background technique
With the propulsion of human industryization process, earth resource is increasingly depleted, and people are being eager to find the same of new energy
When, doubling to pay close attention to can be recycled the existing energy.In addition also environmentally friendly using problem of environmental pollution caused by fossil fuel
Personage and scientists, which are endured to the fullest extent, to denounce.China is since last century the eighties, and while national economy fast development, resource is withered
It exhausts and is also increasingly highlighted the problem of environmental pollution.China accounts for more than half of ultimate resources as coal big country, coal resources,
And coal resources are frequently accompanied by huge waste in exploitation, processing, power generation applications, the three industrial wastes that generate (waste residue,
Waste water is discarded) it is the reform of China's Industrial Green, the recyclable critical issue developed all the time.
Porous material, porous material are a kind of by being mutually communicated or closed hole constitutes the material of network structure, hole
Boundary or surface be made of pillar or plate.Porous material presses the method source world pure chemistry and application of aperture size classification
Tissue is learned, for the research for pushing porous material, recommends above-mentioned technical term.According to the difference of pore size, porous material is again
Micropore (aperture is less than 2nm) material, mesoporous (aperture 2-50nm) material and macropore (aperture is greater than 50nm) material can be divided into.It is more
Porous materials can be made of the carbide of various metals and alloy and refractory metal, nitride, boride and silicide etc..In recent years
Carry out porous carbon materials because its excellent performance receives the concern of industry and new energy field.
Porous carbon materials refer to the carbon materials with Different Pore Structures, and pore size is from being equivalent to receiving for molecular size
Meter level ultrafine micropore is until adapting to microbial growth and movable micron order pore.Porous carbon materials have low-density, low-heat swollen
Swollen coefficient, high heat conductance, high conductivity, high intensity, and there is huge specific surface area, in addition porous carbon materials can also corrosion resistant
Erosion, anti-oxidant, good processability.Therefore, porous carbon materials the purification of gas and liquid, separation and water process,
Air cleaning etc. has been widely used.
In recent years, porous material is played due to its excellent electric conductivity and surface adsorption property in field of energy source materials
Important function as the good carrier of catalyst can greatly accelerate chemical reaction rate, as super capacitor
Device or the electrode material of secondary lithium-sulfur battery show excellent chemical property.
The method of the existing easy sublimate of porous material loading simple substance mainly has:
(1) absorption method: porous material is subjected to briquetting encapsulation composition absorbent packet or adsorption module, utilizes its excellent surface
Adsorption capacity is adsorbed what is passed through containing the easy sublimate element in easy sublimate exhaust gas.Although this method technique letter
It is single, but fail to make full use of porous material high-specific surface area and Kong Rong, it is easily poisoned, loads easy sublimate inefficiency.
(2) exchange of solvent method: by easy sublimate simple substance be dissolved in ethyl alcohol, ether, carbon disulfide, carbon tetrachloride, propane,
In butane, pentane, hexane, hexamethylene, toluene and benzene organic solvent, by above-mentioned solvent impregnated porous material, then by organic solvent
After evaporation, load is precipitated in the porous material in the easy sublimate of simple substance again.But organic solvent is difficult to enter micropore in this method
It is insufficient and not enough uniformly to lead to bear easy sublimate for structure, and how toxic organic solvent is, needed after evaporation reflux condensation mode with
It recycles, leads to complex process, cost is difficult to decline.
(3) heat treating process: the easy sublimate of simple substance and porous material are mixed according to a certain percentage, sealed after stirring ball-milling
In special container, inert atmosphere protection is vacuumized or be passed through, is re-fed into heat-treatment furnace small in 40~150 DEG C of processing 1~8
When, it is heated to 300 DEG C or more and handles 1~3 hour, remove the not compound good extra easy sublimate of simple substance, furnace cooling
To room temperature, the easy sublimate technique of porous material loading simple substance can be completed.This method and process condition is more harsh, when load
Between it is longer, it is difficult to realize automation process.
Summary of the invention
The object of the present invention is to provide the method that one kind loads easy sublimate in the porous material, this method technique letters
Single, at low cost, the high and easy sublimate simple substance of the easy sublimate amount of load is evenly distributed.
The technical scheme adopted by the invention is that a method of easy sublimate, this method are loaded in the porous material
Based on evaporation-cooled device, specific structure are as follows: including sealing container, be communicated with cooling device and inert gas in sealing container
Pipe, cooling device are connected with vacuum pump；
Method particularly includes:
Step 1, the easy sublimate of simple substance is added in sealing container, pretreated porous material is loaded in cooling dress
In setting；
Step 2, it is passed through inert atmosphere into sealing container, and opens vacuum pump, makes to keep negative pressure in sealing container, until complete
The full air excluded in evaporation-cooled device；
Step 3, sealing container is heated, makes the easy sublimate of simple substance by the easy sublimate steam of heat sublimation, and
It is gradually filled with cooling device；
Step 4, cooling device is opened, load certain time is kept according to porous carbon materials quality, load capacity height is obtained, divides
The uniform composite material of cloth.
The features of the present invention also characterized in that
Porous material is porous carbon materials, mesoporous silicon material, zeolite molecular sieve or nickel foam in step 1.
The easy sublimate of simple substance is elemental sulfur, iodine, simple substance naphthalene or alchlor in step 1.
Cooling device is condenser pipe, multitube cooler or cooling tower.
The pretreatment of porous material is dry at 80~100 DEG C after cleaning porous material with deionized water in step 1
10~for 24 hours.
Inert atmosphere is passed through in step 2 into sealing container, and opens vacuum pump, makes to keep negative pressure -0.1 in sealing container
~-10.0Mpa keeps 30s~30min to the complete air excluded in evaporation-cooled device.
Inert atmosphere is nitrogen, helium, neon, argon gas or xenon in step 2.
Heating temperature is 300~500 DEG C in step 3.
The invention has the advantages that the method that the present invention loads easy sublimate in the porous material, has following spy
Point:
(1) environmentally protective, efficient uniform: the present invention after the easy sublimate gasification of simple substance in porous material surface by will coagulate
Solid now to load easy sublimate, reaction temperature is lower (300 DEG C), and no waste generates, and the easy sublimate of gas phase more holds
Easily enter in the multi-stage artery structure of porous material, the structural advantage of porous material is given full play to, to improve porous material
Load capacity, on the other hand since the easy sublimate cooling velocity of gas phase is fast, grain diameter is tiny after solidification, to optimize porous material
Material loads the uniformity coefficient of easy sublimate；
(2) load process is simple, is easily enlarged, automates: in the method for the present invention, after completing instrument layout, substantially not
Manual operation is needed, can be completed.If endlessly easy sublimate source can be provided and the porous material continuously replaced can be real
Now automation continuous batch production.
In conclusion the invention proposes a kind of porous material loading simple substance simple and easy to operate, being easy to automate easily to rise
The method of compound matter, and the composite material of the easy sublimate/porous material obtained has the characteristic that carrying capacity is high, is evenly distributed,
The efficient process that can be used for the industrial waste gas containing easy sublimate can be used for preparing the compound NEW TYPE OF COMPOSITE of uniform high-efficiency
Material.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of evaporation-cooled device used in the method for the present invention；
In figure, 1. sealing containers, 2. inert gas tubes, 3. cooling devices.
Fig. 2 is the hot weight curve of the negative sulphur porous carbon composite obtained in embodiment 1.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The method that the present invention loads easy sublimate in the porous material, this method is based on evaporation-cooled device, such as Fig. 1 institute
Show, specific structure are as follows: including sealing container 1, cooling device 3 and inert gas tube 2, cooling device 3 are communicated in sealing container 1
It is connected with vacuum pump；Cooling device 3 is condenser pipe, multitube cooler or cooling tower；
Method particularly includes:
Step 1, the easy sublimate of simple substance is added in sealing container 1, pretreated porous material is loaded in cooling
In device 3；The pretreatment of porous material be after porous material is cleaned with deionized water dry 10 at 80~100 DEG C~for 24 hours；
Wherein porous material is porous carbon materials, mesoporous silicon material, zeolite molecular sieve or nickel foam；The easy sublimate of simple substance is simple substance
Sulphur, iodine, simple substance naphthalene or alchlor；
Step 2, inert atmosphere (inert atmosphere is nitrogen, helium, neon, argon gas or xenon) is passed through into sealing container 1,
And vacuum pump is opened, make to keep negative pressure -0.1~-10.0Mpa in sealing container 1,30s~30min is kept to exclude evaporation to complete
Air in cooling device；
Step 3, sealing container 1 is carried out being heated to 300~500 DEG C, makes the easy sublimate of simple substance by heat sublimation Yi Sheng
Change material vapors, 1s~10min is kept to make steam full of cooling device 3；
Step 4, cooling device 3 is opened, load 10s~1h is kept according to porous material quality, obtains load capacity height, distribution
Uniform composite material.
Embodiment 1
(1) acetylene black porous carbon materials and used vessel catheter are pre-processed: by 1g acetylene black porous carbon materials and institute
The container and conduit used is put into air dry oven at 80 DEG C dry 10h together after using deionized water to clean, remove surface
Moisture；
(2) 1g elemental sulfur is put into sealing container, 1g acetylene black porous carbon is loaded inside cooling device (condenser pipe)
Material；
(3) it is passed through nitrogen, and opens vacuum pump, adjusting gas cylinder and vacuum pump air valve makes holding -0.1Mpa in sealing container,
Keep 30s to the complete air excluded in whole device；
(4) being heated to temperature to sealing container is 500 DEG C or so, and the elemental sulfur in sealing container is sulphur steaming by heat sublimation
Vapour, sulphur steam enter cooling device under negative pressure driving, 1s are kept to make sulphur steam full of cooling device；
(5) water circulation in condenser pipe is opened, sulphur steam in pipe is rapidly cooled；
(6) negative sulphur technique 10s is kept, can be obtained negative sulfur content height, the uniform composite material of sulphur content cloth.
Fig. 2 is the hot weight curve that porous carbon obtained in embodiment 1 loads elemental sulfur composite material, as can be seen from Fig. 2
Weight change very little, bright sulfur are then gasified totally after porous carbon is heated, and composite material then weightlessness 55% can speculate the composite material
It is middle loaded 55% elemental sulfur.
Embodiment 2
(1) mesoporous silicon material and used vessel catheter are pre-processed: by 100g mesoporous silicon material and used container
Drying at 100 DEG C is put into air dry oven after cleaning with conduit using deionized water together and for 24 hours, removes surface moisture；
(2) 100g iodine is put into sealing container, 100g mesoporous silicon is loaded inside cooling device (multitube cooler)
Material；
(3) it is passed through helium, and opens vacuum pump, adjusting gas cylinder and vacuum pump air valve makes holding-in sealing container
10.0Mpa keeps 30min to the complete air excluded in whole device；
(4) sealing container is heated using electric jacket, heating temperature is 300 DEG C or so, and the iodine in sealing container is heated
Distillation is iodine steam, and iodine steam enters cooling device under negative pressure driving, keeps 10min, makes iodine steam full of cooling device；
(5) open multitube cooler, cooling means is spraying cooling, and cooling medium is salting liquid, to iodine steam in pipe into
Row is quickly cooled down；；
(6) technique 1h is kept, can be obtained load capacity height, the composite material that iodine is evenly distributed.
Embodiment 3
(1) zeolite molecular sieve and used vessel catheter are pre-processed: by zeolite molecular sieve and used container and being led
Pipe is put into air dry oven at 90 DEG C dry 12h together after cleaning using deionized water, remove surface moisture；
(2) 10g simple substance naphthalene is put into sealing container, 50g zeolite molecular sieve is loaded inside cooling device (condenser pipe)；
(3) it is passed through argon gas, and opens vacuum pump, adjusting gas cylinder and vacuum pump air valve makes holding -1.0Mpa in sealing container,
Keep 10min to the complete air excluded in whole device；
(4) sealing container is heated using alcolhol burner, heating temperature is 500 DEG C or so, and the simple substance naphthalene in container is by heat sublimation
For naphthalene steam, naphthalene steam enters cooling device under negative pressure driving, 1min is kept to make naphthalene steam full of cooling device；
(5) condenser pipe is opened, cooling means refrigerant circulation is cooling, and cooling medium is organic solvent；
(6) negative naphthalene technique 30min is kept, can be obtained negative naphthalene amount height, the composite material that naphthalene is evenly distributed.
Embodiment 4
(1) nickel foam and used vessel catheter are pre-processed: nickel foam and used container and conduit use are gone
Drying at 100 DEG C is put into air dry oven after ionized water cleaning together and for 24 hours, removes surface moisture；
(2) 80g alchlor is put into sealing container, 40g nickel foam is loaded inside cooling device；
(3) it is passed through neon, and opens vacuum pump, adjusting gas cylinder and vacuum pump air valve makes to keep negative pressure-in sealing container
2.0Mpa keeps 15min to the complete air excluded in whole device；
(4) sealing container is heated using electric jacket, heating temperature is 300 DEG C or so, alchlor in sealing container by
Heat sublimation is alchlor steam, and alchlor steam enters cooling device under negative pressure driving, 4min is kept to make alchlor
Steam is full of cooling device；
(5) condenser pipe is opened, cooling means is refrigerant circulation cooling etc., and cooling medium is mixture of ice and water；
(6) technique 40min is kept, can be obtained load capacity height, the composite material that alchlor is evenly distributed.
Claims (5)
1. the method that one kind loads easy sublimate in the porous material, which is characterized in that this method is based on evaporation-cooled device,
Specific structure are as follows: including sealing container (1), it is communicated with cooling device (3) and inert gas tube (2) on the sealing container (1),
The cooling device (3) is connected with vacuum pump；
Method particularly includes:
Step 1, the easy sublimate of simple substance is added in sealing container (1), pretreated porous material is loaded in cooling dress
It sets in (3)；
Step 2, inert atmosphere is passed through into sealing container, and opens vacuum pump, make in sealing container keep negative pressure -0.1~-
10.0Mpa keeps 30s~30min to the complete air excluded in evaporation-cooled device；
Step 3, sealing container (1) is heated, makes the easy sublimate of simple substance by the easy sublimate steam of heat sublimation, and by
Gradually it is full of cooling device (3)；
Step 4, cooling device (3) are opened, load certain time is kept according to porous material quality, obtains load capacity height, distribution
Uniform composite material；
Porous material is porous carbon materials, mesoporous silicon material, zeolite molecular sieve or nickel foam in step 1；
The easy sublimate of simple substance is elemental sulfur, iodine, simple substance naphthalene or alchlor in step 1.
2. the method according to claim 1 for loading easy sublimate in the porous material, which is characterized in that the cooling
Device is condenser pipe, multitube cooler or cooling tower.
3. the method according to claim 1 for loading easy sublimate in the porous material, which is characterized in that in step 1
The pretreatment of porous material be after porous material is cleaned with deionized water dry 10 at 80~100 DEG C~for 24 hours.
4. the method according to claim 1 for loading easy sublimate in the porous material, which is characterized in that in step 2
Inert atmosphere is nitrogen, helium, neon, argon gas or xenon.
5. the method according to claim 1 for loading easy sublimate in the porous material, which is characterized in that in step 3
Heating temperature is 300~500 DEG C.
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| CN110544544B (en) * | 2019-09-25 | 2021-07-30 | 中国原子能科学研究院 | Device and method for continuously generating iodine steam |
| CN115382560B9 (en) * | 2022-10-27 | 2023-04-28 | 北京宇极科技发展有限公司 | Block aluminum chloride catalyst, preparation method and application |
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| 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 |
| CN101587951A (en) * | 2008-05-23 | 2009-11-25 | 中国人民解放军63971部队 | Novel carbon-sulfur compound for lithium-sulfur battery |
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| FR2840547B1 (en) * | 2002-06-11 | 2005-03-04 | Commissariat Energie Atomique | METHOD AND DEVICE FOR INCORPORATING A COMPOUND IN PORES OF POROUS MATERIAL AND USES THEREOF |
| CN105304908B (en) * | 2015-10-16 | 2018-07-03 | 广东烛光新能源科技有限公司 | A kind of preparation method of sulfur-bearing electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101587951A (en) * | 2008-05-23 | 2009-11-25 | 中国人民解放军63971部队 | Novel carbon-sulfur compound for lithium-sulfur battery |
| 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 |
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