CN106631153A - Method for loading subliming matters in aerogel material - Google Patents
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- CN106631153A CN106631153A CN201611241817.3A CN201611241817A CN106631153A CN 106631153 A CN106631153 A CN 106631153A CN 201611241817 A CN201611241817 A CN 201611241817A CN 106631153 A CN106631153 A CN 106631153A
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Abstract
The invention relates to a method for loading subliming matters in an aerogel material. The method comprises the following steps: putting a subliming elementary substance into the bottom of a piston sealing cylinder, stacking the aerogel material onto the upper part and putting in a piston; discharging air in the cylinder and the aerogel material, and then introducing inert gas from a cylinder outlet; sealing the cylinder outlet, quickly pushing the piston and increasing the temperature of the inert gas in the cylinder under the effect of sudden compression, thereby heating and subliming the subliming elementary substance and causing the subliming elementary substance enter into a pore channel of the aerogel material; quickly drawing the piston to the initial length of the aerogel material, reducing the temperature of the inert gas under the effect of volume expansion, coagulating the gas-phase subliming matters into nanometer-scale particles following the reducing of the temperature and uniformly dispersing the nanometer-scale particles into the pore channel of the aerogel material; and acquiring the aerogel material with high subliming matter load. According to the method provided by the invention, the load is high and the subliming matters are uniformly distributed. The method can be used for treating the industrial waste gas containing the subliming matters and preparing a uniform compound material.
Description
Technical field
The invention belongs to field of environment protection or field of compound material, and in particular to one kind loads easily distillation in aerogel material
The method of material.
Background technology
With the propulsion of human industryization process, earth resource increasingly depleted, people are being eager to find the same of novel energy
When, double to pay close attention to the reusable edible to the existing energy.It is also environmentally friendly using problem of environmental pollution caused by fossil fuel in addition
Personage and scientists are endured to the fullest extent and are denounced.Since the last century the eighties, while national economy is fast-developing, resource is withered for China
Exhaust and also increasingly highlighted with 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 discarded object in exploitation, processing, in power generation applications, three industrial wastes that it is produced (waste residue,
It is waste water, discarded) it is all the time China's Industrial Green reform, the key issue of development capable of circulation.
Aerogel material, is also called xerogel.When gel sloughs most of solvent, content liquid in gel is set to contain than solid
The medium being full of in amount much less, or the space net structure of gel is gas, and appearance is in solid-like, and this is xerogel,
Referred to as aeroge.Aeroge is a kind of solid matter form, one of solid of world's upper density very little.Density is often stood for 3 kilograms
Square rice.General common aeroge is silica aerogel, its earliest by American science worker Kistler in 1931 because friendly with it
Bet and be obtained.The species of aeroge is a lot, there is silicon systems, carbon system, sulphur system, metal oxide system, metal system etc..Aerogel material
All there is important researching value in fractional structure field, heat-barrier material research field, acoustic material research field.
In recent years, in energy storage material field, carbon aerogels are after fibrous activated carbon as the porous material of novel conductive
A kind of novel carbon material for growing up later, it has very big specific surface area (600-1000m2/ kg) and high conductivity
(10-25s/cm).And, the wide (0.05-1.0g/cm of variable density scope3).Appropriate electrolysis is such as filled with its Micro-v oid
Liquid, can make Novel rechargeable battery, and it has, and storing up electricity capacity is big, internal resistance is little, lightweight, charging and discharging capabilities strong, can be multiple
The excellent specific properties such as reuse, preliminary experimental results show：The charging capacity of carbon aerogels is up to 3 × 104/kg2, power density is
7kw/kg, repeated charge is functional, is widely used in the every field such as electrochemistry, catalysis and environmental protection.
The method of the easy sublimate of existing aerogel carried simple substance mainly has：
(1) absorption method：Aerogel material is carried out into briquetting encapsulation composition absorbent packet or adsorption module, using its excellent table
Face adsorption capacity is adsorbed the easy sublimate element in passing through containing easy sublimate waste gas.Although the method technique is simple
It is single, but fail to make full use of aeroge high-specific surface area and pore volume, easily poisoning loads easy sublimate inefficiency.
(2) exchange of solvent method：By easy sublimate simple substance be dissolved in ethanol, ether, carbon disulfide, carbon tetrachloride, propane,
In butane, pentane, hexane, hexamethylene, toluene and benzene organic solvent, by above-mentioned solvent impregnated aerogel material, then will be organic molten
After agent evaporation, the easy sublimate of simple substance is separated out and is supported in aerogel material again.But organic solvent is difficult to enter in the method
Microcellular structure, causes negative easy sublimate insufficient and not uniform enough, and how toxic organic solvent is, and returned cold is needed after evaporation
Coagulate to recycle, cause complex process, cost to be difficult to decline.
(3) chemical method：By the reaction raw materials dissolving of easy sublimate in a solvent, then aerogel material is dispersed in into this molten
In agent, provocative reaction under certain condition, reaction generates the easy sublimate particulate load of simple substance in aerogel material.But the party
Organic solvent is difficult to enter microcellular structure in method, causes easy sublimate load insufficient and not uniform enough, and need to be through control
There is chemical reaction, reaction precision is difficult to control to condition, complex process, high cost.
(4) heat treating process：The easy sublimate of simple substance and aerogel material are mixed according to a certain percentage, it is close after stirring ball-milling
In being encapsulated in special container, inert atmosphere protection is vacuumized or be passed through, be re-fed into heat-treatment furnace little in 40-150 DEG C of process 1-8
When, more than 300 DEG C process 1-3 hours are heated to, remove and be not combined the good easy sublimate of unnecessary simple substance, cool to the furnace
Room temperature, you can complete the easy sublimate technique of aerogel carried simple substance.This method process conditions are more harsh, load time compared with
It is long, it is difficult to realize automation process.
The content of the invention
It is an object of the invention to provide a kind of method that easy sublimate is loaded in aerogel material, the method load is easily
Sublimate amount is high and easily sublimate simple substance is evenly distributed, environment-friendly and green.
The technical solution adopted in the present invention is, a kind of method that easy sublimate is loaded in aerogel material, specifically
Implement according to following steps：
Step 1, by the easy sublimate of simple substance piston seal cylinder bottom is put into, and the easy sublimate top of simple substance stacks airsetting
Glue material, loads piston；
Step 2, discharges the air in cylinder and in aerogel material, is then passed through inert gas by cylinder outlet；
Step 3, sealing cylinder outlet, quick pushing piston, the inert gas in cylinder heats up due to compressing suddenly, causes
Easy sublimate simple substance is made by heat sublimation, and under piston pressure among the duct of aerogel material；
Step 4, quick pull piston to aerogel material initial length, inert gas because of volumetric expansion temperature drop, with
The decline of temperature, the easy sublimate of gas phase condenses to form nano-scale particle, and is dispersed in the duct of aerogel material；
Step 5, repeats 2-4 step operations, that is, obtain the aerogel material of high easily sublimate load capacity.
Of the invention the characteristics of, also resides in,
Aerogel material and the mass ratio of the easy sublimate of simple substance are 1 in step 1：4-5.
Aerogel material is carbon aerogels material or Silica Aerogels.
The easy sublimate of simple substance is one or more mixture in sulphur, iodine, naphthalene or alchlor.
Inert gas is one or more mixture in nitrogen, helium, neon, argon gas or xenon in step 2.
Inert gas compression ratio is 2-10 in cylinder in step 3.
Piston pushing speed is 0.2-1m/s in step 3.
The invention has the beneficial effects as follows, the method that the present invention loads easy sublimate in aerogel material, with following
Feature：
(1) environmental protection：The present invention is realized after by the easy sublimate gasification of simple substance in aerogel material internal condensate
Easy sublimate is loaded, without the need for thermal source heating, is produced without discarded object；
(2) easily sublimate loads efficient uniform：Aerogel material inner air is discharged before load, is more beneficial for gas phase
Easily sublimate is entered in the multi-stage artery structure of aeroge, gives full play to the structural advantage of aerogel material, on the other hand by
Fast in the easy sublimate cooling velocity of gas phase, grain diameter is tiny after solidification, so as to optimize aerogel carried easy sublimate
Uniformity coefficient；
(3) simple process is controllable：Carrying method of the present invention is simple, and by controlling push-and-pull number of times airsetting glue material can be just adjusted
The load capacity of material, in addition the inventive method is easily enlarged, automates, if can provide endlessly easy sublimate source and connect
The continuous aerogel material changed is capable of achieving automation continuous batch production.
In sum, the present invention propose it is a kind of it is simple and easy to operate, be easy to automate aerogel material load simple substance it is easy
The method of sublimate, and the easy sublimate/aerogel composite for obtaining has the characteristic that load capacity is high, be evenly distributed,
The invention can be used for the efficient process of the industrial waste gas containing easy sublimate, it is also possible to for preparing compound new of uniform high-efficiency
Type composite.
Description of the drawings
Fig. 1 is the process schematic representation of the inventive method；
Fig. 2 is the surface sweeping electron microscope of carbon gel rubber material used in embodiment 1；
Fig. 3 is the thermogravimetric curve figure of the elemental sulfur/carbon aerogel composite material prepared by embodiment 1.
Specific embodiment
With reference to the accompanying drawings and detailed description the present invention is described in detail.
The present invention easy sublimate is loaded in aerogel material method, concrete technology as shown in figure 1, specifically according to
Lower step is implemented：
Step 1, by the easy sublimate of simple substance piston seal cylinder bottom is put into, and the easy sublimate top of simple substance stacks airsetting
Glue material, loads piston；Aerogel material is 1 with the mass ratio of the easy sublimate of simple substance：4-5；Aerogel material is carbon airsetting
Glue material or Silica Aerogels；The easy sublimate of simple substance is one or more mixture in sulphur, iodine, naphthalene or alchlor；
Step 2, discharges the air in cylinder and in aerogel material, is then passed through inert gas by cylinder outlet (lazy
Property gas be nitrogen, helium, neon, argon gas or xenon in one or more mixture), until in cylinder inert gas compression
Than for 2-10；
Step 3, sealing cylinder outlet, with pushing speed as the quick pushing pistons of 0.2-1m/s, the inert gas in cylinder
Heat up due to compressing suddenly, cause easy sublimate simple substance by heat sublimation, and into aerogel material under piston pressure
Among duct；
Step 4, quick pull piston to aerogel material initial length, inert gas because of volumetric expansion temperature drop, with
The decline of temperature, the easy sublimate of gas phase condenses to form nano-scale particle, and is dispersed in the duct of aerogel material；
Step 5, repeats 2-4 step operations, that is, obtain the aerogel material of high easily sublimate load capacity.
Embodiment 1
(1) used vessel catheter is pre-processed：The cylinder for being used and piston are used after deionized water cleaning in the lump
It is put into air dry oven at 80 DEG C and is dried 10h, removes surface moisture；
(2) 5g sublimed sulfurs are put into piston seal cylinder bottom, 1g carbon aerogels materials is stacked thereon, load piston；
(3) pushing piston causes cylinder bottom, thoroughly discharges the air in cylinder and in carbon aerogels, and cylinder outlet is connected
Nitrogen, it is 2 that pull piston is filled with nitrogen to compression ratio；
(4) sealing cylinder outlet, quick pushing piston, pushing speed is 0.2m/s, and the nitrogen in cylinder due to pressing suddenly
Contract and heat up, cause sublimed sulfur by heat sublimation, and under piston pressure among the duct of carbon aerogels material；
(5), to carbon aerogels material initial length, nitrogen is because of volumetric expansion temperature drop, gaseous state distillation for quick pull piston
Sulphur condenses to form nano-scale particle, and is dispersed in the duct of carbon aerogels material；
(6) piston is pulled out, takes out composite, that is, obtain the sulphur/carbon aerogel composite material of high capacity amount.
Fig. 2 is the stereoscan photograph of carbon aerogels used in embodiment 1, and as can be seen from Fig. 2 carbon aerogels are three-dimensional
Self-assembled structures, with a large amount of multi-stage artery structures, can effectively adsorb volatile substances.
Fig. 3 is the thermogravimetric curve of sulphur/carbon aerogel composite material that embodiment 1 is obtained and carbon aerogels material, from Fig. 3
The load sulfur content of the visible prepared sulphur/carbon aerogel composite material of contrast reaches 75%.
Embodiment 2
(1) used vessel catheter is pre-processed：The cylinder for being used and piston are used after deionized water cleaning in the lump
It is put into air dry oven at 100 DEG C and is dried 24h, removes surface moisture；
(2) 20g iodines are put into piston seal cylinder bottom, 5g Silica Aerogels is stacked thereon, load piston；
(3) pushing piston causes cylinder bottom, thoroughly discharges the air in cylinder and in silica aerogel, and cylinder outlet is connected
Argon gas, it is 10 that pull piston is filled with argon gas to compression ratio；
(4) sealing cylinder outlet, quick pushing piston, pushing speed is 1m/s, and the argon gas in cylinder due to compressing suddenly
And heat up, iodine is caused by heat sublimation, and under piston pressure among the duct of Silica Aerogels；
(5), to aerogel material initial length, argon gas is because of volumetric expansion temperature drop, gaseous elemental iodine for quick pull piston
Condensation forms nano-scale particle, and is dispersed in the duct of Silica Aerogels；
(6) repeat (3-5) step to operate five times, pull out piston, take out composite, that is, obtain the iodine/silicon gas of high capacity amount
Gel complex material.
Embodiment 3
(1) used vessel catheter is pre-processed：The cylinder for being used and piston are used after deionized water cleaning in the lump
It is put into air dry oven at 90 DEG C and is dried 16h, removes surface moisture；
(2) 10g simple substance naphthalenes are put into piston seal cylinder bottom, 2g carbon aerogels materials is stacked thereon, load piston；
(3) pushing piston causes cylinder bottom, thoroughly discharges the air in cylinder and in carbon aerogels, and cylinder outlet is connected
Nitrogen argon gas gaseous mixture, it is 6 that pull piston is filled with nitrogen argon gas gaseous mixture to compression ratio；
(4) sealing cylinder outlet, quick pushing piston, pushing speed is 0.6m/s, the nitrogen argon gas gaseous mixture in cylinder
Heat up due to compressing suddenly, cause simple substance naphthalene by heat sublimation, and under piston pressure into carbon aerogels material duct it
In；
(5) quick pull piston is to aerogel material initial length, nitrogen argon gas gaseous mixture because of volumetric expansion temperature drop,
Gaseous elemental naphthalene condenses to form nano-scale particle, and is dispersed in the duct of carbon aerogels material；
(6) repeat (3-5) step to operate three times, pull out piston, take out composite, you can obtain the naphthalene/carbon of high capacity amount
Aerogel composite.
Claims (7)
1. a kind of method that easy sublimate is loaded in aerogel material, it is characterised in that specifically implement according to following steps：
Step 1, by the easy sublimate of simple substance piston seal cylinder bottom is put into, and the easy sublimate top of simple substance stacks airsetting glue material
Material, loads piston；
Step 2, discharges the air in cylinder and in aerogel material, is then passed through inert gas by cylinder outlet；
Step 3, sealing cylinder outlet, quick pushing piston, the inert gas in cylinder heats up due to compressing suddenly, causes easily
Sublimate simple substance receives heat sublimation, and under piston pressure among the duct of aerogel material；
Step 4, quick pull piston to aerogel material initial length, inert gas because of volumetric expansion temperature drop, with temperature
The decline of degree, the easy sublimate of gas phase condenses to form nano-scale particle, and is dispersed in the duct of aerogel material；
Step 5, repeats 2-4 step operations, that is, obtain the aerogel material of high easily sublimate load capacity.
2. the method that easy sublimate is loaded in aerogel material according to claim 1, it is characterised in that step 1
Middle aerogel material is 1 with the mass ratio of the easy sublimate of simple substance：4-5.
3. the method that easy sublimate is loaded in aerogel material according to claim 1 and 2, it is characterised in that institute
Aerogel material is stated for carbon aerogels material or Silica Aerogels.
4. the method that easy sublimate is loaded in aerogel material according to claim 1 and 2, it is characterised in that single
The easy sublimate of matter is one or more mixture in sulphur, iodine, naphthalene or alchlor.
5. the method that easy sublimate is loaded in aerogel material according to claim 1, it is characterised in that step 2
Middle inert gas is one or more mixture in nitrogen, helium, neon, argon gas or xenon.
6. the method for loading easy sublimate in aerogel material according to claim 1 or 5, it is characterised in that step
Inert gas compression ratio is 2-10 in cylinder in rapid 3.
7. the method that easy sublimate is loaded in aerogel material according to claim 1, it is characterised in that step 3
Middle piston pushing speed is 0.2-1m/s.
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Cited By (4)
| 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 |
| 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 |
| 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 |
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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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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