CN1843958A - Method for preparing globular silver carried organic aerogel and carbon aerogel particle - Google Patents
Method for preparing globular silver carried organic aerogel and carbon aerogel particle Download PDFInfo
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- CN1843958A CN1843958A CN 200610035097 CN200610035097A CN1843958A CN 1843958 A CN1843958 A CN 1843958A CN 200610035097 CN200610035097 CN 200610035097 CN 200610035097 A CN200610035097 A CN 200610035097A CN 1843958 A CN1843958 A CN 1843958A
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Abstract
The invention relates to a method for preparation of spherical organic aerogel carrying silver and charcoal aerogel grain.Selecting silver complex as catalyst, resorcin and formaldehyde as reaction monomer, water as dissolvent, to prepare pnenolic aldehyde solution containing silver; using heterophase sedimentation method, dropping continuously said solution above oil phase column before froming gel, drops forming organic gel grain when settling at the bottom of the column, by aging, scouring and desiccation, to get organic aerogel grain; then charring it in inert atmosphere, to get spherical organic aerogel grain. The grain obtained is smooth on surface, and the nanometer silver particle inside it is even in distribution, with abundant micropore and mesopore in gel, BET specific surface area of more than 400-500m2/g; furthermore, the method is easy and rapid, with controlled size of gel particle, so it can realize commercial manufacture. It is anticipated that cellular charcoal material carring silver has good character of adsorption and antibiosis, and make silver dissolve out constantly, so it has a fine application prospect in water purification and treatment.
Description
Technical field
The present invention relates to a kind of method that adopts the out-phase settling process to prepare globular silver carried organic aerogel and carbon aerogel particle.
Background technology
Porous carbon material is because its huge specific surface area and excellent absorption property have application widely as adsorption and separation material in purification of waste water is handled.Not only require this porous carbon material that excellent absorption property is arranged when being applied to drinking water treatment, and should have anti-microbial property.For this reason, forefathers metal-silver-doped porous carbon material (as Ag/AC, Ag/ACF) preparation and done many research work in the drink water purifying application facet.Although the active carbon loading silver fiber has the excellent antibiotic performance, also there is very big problem aspect antiscour and the silver-colored stripping.Charcoal-aero gel is a kind of novel nano porous carbon material with three-dimensional net structure that is formed by connecting by nano level spherical shape charcoal particle.Because this material has low density, high-specific surface area, abundant constructional features such as mesopore, can be used as a kind of good porous support, and various active adulterants are loaded in the charcoal-aero gel.
The adulterated charcoal-aero gel preparation method of metal current mainly contains pickling process, ion exchange method and sol-gel method.Pickling process is that the method that the organic aerogel of employing constant pressure and dry floods in the water-soluble metal salts solution prepares metal-doped charcoal-aero gel.Recently, Wu Dingcai etc. successfully prepare the block organic aerogel of exsiccant under the condition of normal pressure, and on this working foundation, Fu Ruowen etc. adopt Ag-containing solution dipping organic aerogel, and the block silver-colored charcoal-aero gel that carries is prepared in charing then.Be used for the application of water treatment anti-biotic material, have good antibiotic enduring quality and security.
Year silver-colored carbon aerogel material of immersion process for preparing reunite owing to silver ions in steeping process easily reduces to grow, thereby silver particles size homogeneity is slightly poor.In addition, from angle of practical application, a block year silver-colored charcoal-aero gel must be ground into sizeable particle earlier before column packed, and the granular size that forms in crushing process is inhomogeneous, and the silver-colored particle in the gel network easily comes out after pulverizing, comes off easily after current scour.The adventitia densification of spherical gel particles, the silver particles of load is coated in the gel-film, and stronger erosion resistibility and lower silver-colored stripping quantity are arranged.For this reason, the preparation method who studies globular silver carried carbon aerogel particle has great application prospect.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing globular silver carried organic aerogel and carbon aerogel particle.
The inventive method is short according to the argentiferous phenolic aldehyde solution gel transitional period, become the fireballing characteristic of glue, with the silver complex is catalyzer, and Resorcinol and formaldehyde are raw material, is mixed with argentiferous phenolic aldehyde solution, adopt the out-phase settling process, make drop gelation in the settled process in the oil phase post, form gel particle, through aging, washing, constant pressure and dry, obtain the organic aerogel particle, and then charing makes globular silver carried carbon aerogel particle.
The method that the present invention prepares silver carried organic aerogel and carbon aerogel particle is: with AgNO
3Being mixed with silver complex, is reaction monomers with Resorcinol and formaldehyde, and water as solvent is mixed with argentiferous phenolic aldehyde solution; Each composition proportion is: Resorcinol R/Ag=10～100 mass ratioes, and Resorcinol R/ formaldehyde F=0.4～0.6 mol ratio, the volume ratio of the quality R of Resorcinol and water W is 0.4～1.5g/ml; The argentiferous phenolic aldehyde solution for preparing at room temperature place or preheating in 25～55 ℃ of water-baths (preheating can be shortened the time that solution becomes milk sap) when solution becomes near milk sap, adopt the out-phase settling process, above the oil phase post, splash into continuously, oil phase column temperature scope is 65～95 ℃ (being preferably 80～95 ℃), when droplet settling forms organic gel particle during to the oil phase column bottom, it is airtight in the reaction flask that the organogel particle is packed into, under 75～85 ℃, wear out and (be generally 2～7 days) more than 2 days, take out the oil phase in back water or the organic solvent flush away gel particle, seasoning or heating, drying obtain the organic aerogel particle under condition of normal pressure; Afterwards, charing gets globular silver carried carbon aerogel particle in inert atmosphere.
In the invention described above method, the argentiferous phenolic aldehyde solution for preparing at room temperature is placed to the time that solution becomes near milk sap and was generally 2～60 minutes, is preheated to the time that solution becomes near milk sap to be generally 2～30 minutes in water-bath; The length of time and the silver content of solution are inversely proportional to.
According to the invention described above method, the coordination agent of described silver complex is preferably: Na
2S
2O
3/ Na
2SO
3(Ag/Na
2S
2O
3=0.35 mol ratio, Ag/Na
2SO
3Or Na=0.5 mol ratio),
2S
2O
3/ NH
3H
2O (Ag/Na
2S
2O
3=0.35 mol ratio, Ag/NH
3H
2O=0.25～0.5 mol ratio).
According to the invention described above method, the oil phase kind of described oil phase post can be that density range is at 0.75～1.0g/cm
3, viscosity (is generally 0.5～140mPas) oils, for example: vacuum pump oil, silicone oil, peanut oil or whiteruss etc. greater than 0.5mPas.Described oil phase post height is generally 1～3m.
According to the invention described above method, the described sol solution that splashes into continuously above the oil phase post normally adopts injection system to splash into, and injects used pinhole diameter and is generally 0.5～2.5mm.
According to the invention described above method, the time of described organogel particle seasoning was generally 2～5 days; The temperature of heating, drying is generally 60～110 ℃, and the time is 4～24 hours.
According to the invention described above method, the temperature of described organic aerogel particle charing is generally 600～1100 ℃, and carbonization time is 2～3 hours.
In the methods of the invention, silver ions and Sulfothiorine coordination reducing the reduction potential of silver, are deposited by the phenolic aldehyde solution reduction avoiding, silver can be entrained in the gel structure equably.When the density argentiferous phenolic aldehyde solution bigger than oil phase splashes in the oil phase, formed the drop of certain size, in settling process, be subjected to the effect of oil phase frictional force and slowly descend.When settling time during greater than gelation time, drop promptly forms gel particle before reaching the oil phase column bottom.The size of gel particle can be controlled by the aperture of sample introduction speed and injection needles.In the methods of the invention, silver is not only as catalyzer but also as the doping composition of gel.
Preparation-obtained year silver-colored carbon aerogel particle smooth surface of the inventive method, inner nano silver particles is evenly distributed (as shown in Figure 1); Gel inside has abundant microporous, mesopore and a small amount of macropore, and the BET specific surface area can reach 400～500m
2More than/the g.The preparation method is easy, and fast, the gel particle controlled amount can realize suitability for industrialized production.
The present invention adopts the out-phase settling process to prepare globular silver carried organic aerogel and carbon aerogel particle, by the direct dopen Nano silver particles equably in charcoal-aero gel of sol-gel process, silver particles is embedded in the three-dimensional manometer network structure to be unlikely to come off, expect that this year silver-colored raw material of wood-charcoal material can keep good absorption anti-microbial property, and can make the lasting stripping of silver, aspect the water purifying treatment good prospects for application arranged.
Description of drawings
Fig. 1 is the globular silver carried organic aerogel (A) and charcoal-aero gel (B) the particle synoptic diagram of the inventive method preparation.
Fig. 2 is the used a kind of reaction unit synoptic diagram of the inventive method.Wherein each mark is depicted as: 1---sampler (can be syringe), 2---the oil pump interface, 3---steam entry or hot water outlet, 4---sleeve pipe, 5---the hollow glass post, 6---steam outlet or hot water inlet, 7---the oil phase outlet, 8---the oil bath heating and temperature controlling device, 9---three-necked bottle, 10---magnetic stirring apparatus, 11---storage tank, 12---the oil phase inlet.
Embodiment
Below the present invention is further illustrated by drawings and Examples.Among each embodiment, each composition proportion R/Ag is a mass ratio; Ag/Na
2SO
3, Ag/NH
3H
2O and R/F are mol ratio; R/W is that mass/volume is than (g/ml).
The inventive method can realize by reaction unit shown in Figure 2.As shown in Figure 2, this reaction unit is by the hollow glass post 5 of tyre sleeve pipe 4 (also can be without sleeve pipe 4, realize heat tracing and be placed on the hollow glass post with electric mantle), three-necked bottle 9, syringe 1, oil bath heating and temperature controlling device 8, magnetic stirring apparatus 10 and storage tank 11 are formed.The general height of hollow glass post is 1-3m, internal diameter 2～5cm.Operating process is: close the switch of oil phase outlet 7 earlier, connect storage tank, start the oil pump that connects oil pump interface 2 then, the oil phase of extracting storage tank enters the hollow glass post, is evacuated to the switch of closing oil phase inlet 12 behind the certain altitude, closes oil pump.Feed water vapour (from top to bottom) from steam entry or hot water outlet 3 in sleeve pipe, or feed hot water (from lower to upper) from steam outlet or hot water inlet 6 in sleeve pipe, the heating oil phase is to certain temperature; The heating unit of control below oil bath simultaneously makes homo(io)thermism.Start magnetic stirring apparatus.Argentiferous phenolic aldehyde solution is splashed into continuously from oil phase post top, is deposited to back, oil column bottom and forms gel particle, and below be subjected to the magnetic stirring apparatus effect in the three-necked bottle and be in whipped state, to prevent the gel particle aggegation together.After reaction finishes, slowly open the oil phase gate out switch, emit oil phase, take out the gel particle in the three-necked bottle, it is airtight in the reaction flask to pack into, aging certain hour under 75～85 ℃ takes out the oil phase in back water or the organic solvent flush away gel particle, and seasoning or heating, drying obtain the organic aerogel particle under condition of normal pressure; Afterwards, charing obtains globular silver carried carbon aerogel particle in inert atmosphere.Various embodiments of the present invention are carried out with reference to said apparatus and process.
Embodiment 1.R/Ag=20, Ag/Na
2SO
3=0.5, R/F=0.5, R/W=1.5. adopts device as shown in Figure 2, and the hollow glass post is high 2 meters, internal diameter 2.5cm, and oil phase is vacuum pump oil (density 0.899g/cm
3, viscosity 7.970mPas), in sleeve pipe, feed the water vapour heating, make the oil phase column temperature keep 95 ℃, heated constant temperature is started magnetic stirring apparatus at 85 ℃ in the three-necked bottle of below.With 1.605gAgNO
3Join 2.40gNa
2SO
3The aqueous solution in the dissolving after, add 7.00gNa again
2S
2O
35H
2O is mixed with silver complex solution, adds 20g Resorcinol, 25.2ml formaldehyde in silver complex solution, and total add-on of deionized water is 13.20ml in the solution, is mixed with argentiferous phenolic aldehyde solution.With this argentiferous phenolic aldehyde solution in 25 ℃ of water-baths about preheating 5min, when treating that solution becomes near milk sap, splash into continuously above the oil phase post with the mode of No. 4.5 syringe needles (pinhole diameter is 1.3mm) with injection, when arriving the oil phase column bottom, droplet settling forms the canescence gel particle, it is airtight in the reaction flask that gel particle is packed into, in 85 ℃ of silicone oil baths, wore out 4 days, take out the oil phase in the water flush away gel of back; Seasoning 3 days obtains garnet silver carried organic aerogel particle.This silver carried organic aerogel is placed in the charring furnace, and feeding flow is the N of 800ml/min
2Gas, be warmed up to 900 ℃ with the speed of 5 ℃/min after, kept 3 hours in this temperature, making diameter is about 1.6mm, of uniform size year silver-colored carbon aerogel particle, its BET specific surface area reaches 328m
2/ g.
Embodiment 2.R/Ag=50, Ag/NH
3H
2O=0.5, R/F=0.4, R/W=0.9. adopt with example 1 device, are oil phase (density 0.821g/cm with the whiteruss
3, viscosity 0.51mPas), in sleeve pipe, feed the water vapour heating, make the oil phase column temperature keep 95 ℃, heated constant temperature is started magnetic stirring apparatus at 85 ℃ in the three-necked bottle of below.Get Na
2S
2O
35H
2O 1.350g is dissolved in the 2.5mL deionized water; Take by weighing 0.308gAgNO
3Be dissolved in the 1mL deionized water, add 0.13ml ammoniacal liquor and be made into silver ammino solution, join the Na that has prepared again
2S
2O
3In the solution, get the silver complex solution A, take by weighing the 10g Resorcinol, be dissolved in the 8mL deionized water and get solution B; At last A solution is joined in the 15.62ml formaldehyde, join again in the solution B, be mixed with argentiferous phenolic aldehyde solution.With this argentiferous phenolic aldehyde solution in 25 ℃ of water-baths about preheating 10min, when treating that solution becomes near milk sap, splash into continuously above the oil phase post with the mode of No. 4.5 syringe needles (pinhole diameter is 1.3mm) with injection, when arriving the oil phase column bottom, droplet settling forms the canescence gel particle, it is airtight in the reaction flask that gel particle is packed into, in 85 ℃ of silicone oil baths, wore out 2 days, use the oil phase in the toluene flush away gel after taking out.Directly dried by the fire 24 hours down at 60 ℃, making average diameter of particles is about 2.8mm, silver carried organic aerogel particle of uniform size.
Embodiment 3.R/Ag=10, Ag/NH
3H
2O=0.5, R/F=0.6, R/W=0.4. adopts device as shown in Figure 2, with dimethyl silicone oil (density 0.999g/cm
3, viscosity 138.3mPas) and be oil phase, the hollow glass post is high 1 meter, internal diameter 5cm, feeds the water vapour heating in sleeve pipe, makes the oil phase column temperature keep 95 ℃, and heated constant temperature is started magnetic stirring apparatus at 85 ℃ in the three-necked bottle of below.Get Na
2S
2O
35H
2O6.565g is dissolved in the 8mL deionized water.Take by weighing 1.573gAgNO
3Be dissolved in the 4mL deionized water, be made into silver ammino solution, transfer to the Na that has prepared again with 0.65ml ammoniacal liquor
2S
2O
3In the solution, get the silver complex solution A, take by weighing the 10g Resorcinol, be dissolved in the 13mL deionized water and get solution B.At last A solution is joined in the 10.42mL formaldehyde, transfer to again in the solution B, be mixed with argentiferous phenolic aldehyde solution.This argentiferous phenolic aldehyde solution room temperature is transferred and is put about 2 minutes, when treating that solution becomes near milk sap, not adding syringe needle (aperture 2.5mm) with the 50ml syringe splashes into above the oil phase post continuously, when arriving the oil phase column bottom, droplet settling forms the canescence gel particle, it is airtight in the reaction flask that gel particle is packed into, in 75 ℃ of silicone oil baths, wore out 7 days, use the oil phase in the acetone flush away gel after taking out.After the seasoning 2 days, baking is 4 hours in 110 ℃ of baking ovens, and obtaining average diameter of particles is about 4.2mm, silver carried organic aerogel particle of uniform size.
Embodiment 4:R/Ag=60, Ag/NH
3H
2O=0.5, R/F=0.45, R/W=0.9. adopt with example 1 device, are oil phase with the vacuum pump oil, feed the water vapour heating in sleeve pipe, make the oil phase column temperature keep 95 ℃, and heated constant temperature is started magnetic stirring apparatus at 85 ℃ in the three-necked bottle of below.Get Na
2S
2O
35H
2O 1.135g is dissolved in the 2.5mL deionized water.Take by weighing 0.259gAgNO
3Be dissolved in the 1mL deionized water, be made into silver ammino solution, transfer to the Na that has prepared again with 0.11ml ammoniacal liquor
2S
2O
3In the solution, get the silver complex solution A; Take by weighing the 10g Resorcinol, be dissolved in the 8mL deionized water, get solution B.At last A solution is joined in the 14.00mL formaldehyde, transfer to again in the solution B, be mixed with argentiferous phenolic aldehyde solution.With this argentiferous phenolic aldehyde solution in 45 ℃ of water-baths about preheating 5min, when treating that solution becomes near milk sap, splash into continuously above the oil phase post with the mode of No. 12 syringe needles (pinhole diameter is 1.8mm) with injection, when arriving the oil phase column bottom, droplet settling forms the grey gel particle, it is airtight in the reaction flask that gel particle is packed into, in 85 ℃ of silicone oil baths, wore out 4 days, take out the oil phase in the water flush away gel of back.Directly dried by the fire 24 hours down at 60 ℃, obtaining average diameter of particles is about 2.8mm, silver carried organic aerogel particle of uniform size.Silver carried organic aerogel is placed in the charring furnace, and feeding flow is the N of 800ml/min
2Gas, be warmed up to 900 ℃ with the speed of 5 ℃/min after, kept 3 hours in this temperature, making diameter is about 2.2mm, S
BET=409m
2/ g, of uniform size year silver-colored carbon aerogel particle.
Embodiment 5:R/Ag=70, Ag/NH
3H
2O=0.5, R/F=0.5, R/W=0.9. adopt with example 1 device, are oil phase with the vacuum pump oil, feed the water vapour heating in sleeve pipe, make the oil phase column temperature keep 95 ℃, and heated constant temperature is started magnetic stirring apparatus at 85 ℃ in the three-necked bottle of below.Get Na
2S
2O
35H
2O0.972g is dissolved in the 2.5mL deionized water.Take by weighing 0.222gAgNO
3Be dissolved in the 1mL deionized water, be made into silver ammino solution, join the Na that has prepared again with 0.09ml ammoniacal liquor
2S
2O
3In the solution, get the silver complex solution A.Take by weighing the 10g Resorcinol, be dissolved in the 8mL deionized water, get solution B.At last A solution is joined in the 12.50mL formaldehyde, join again in the solution B, be mixed with argentiferous phenolic aldehyde solution.With this argentiferous phenolic aldehyde solution in 45 ℃ of water-baths about preheating 8min, when treating that solution becomes near milk sap, above the oil phase post, splash into continuously in the mode of injecting with No. 4.5 syringe needles, when arriving the oil phase column bottom, droplet settling forms the grey gel particle, it is airtight in the reaction flask that gel particle is packed into, in 85 ℃ of silicone oil baths, wore out 4 days, take out the oil phase in the water flush away gel of back.Directly dried by the fire 24 hours down at 60 ℃, obtain the silver carried organic aerogel that average diameter of particles is (as Figure 1A) about 2.0mm.Silver carried organic aerogel is placed in the charring furnace, and feeding flow is the N of 800ml/min
2Gas, be warmed up to 900 ℃ with the speed of 5 ℃/min after, kept 3 hours in this temperature, making diameter is (as Figure 1B) about 1.6mm, S
BET=428m
2/ g, of uniform size year silver-colored carbon aerogel particle.
Embodiment 6:R/Ag=100, Ag/NH
3H
2O=0.25, R/F=0.45, R/W=0.9. device as shown in Figure 2, with the vacuum pump oil is oil phase, and the hollow glass post is high 3 meters, internal diameter 2.5cm, feeds the water vapour heating in sleeve pipe, make the oil phase column temperature keep 95 ℃, heated constant temperature is started magnetic stirring apparatus at 85 ℃ in the three-necked bottle of below.Get Na
2S
2O
35H
2O1.135g is dissolved in the 2.5mL deionized water.Take by weighing 0.295g AgNO
3Be dissolved in the 1mL deionized water, be made into silver ammino solution, transfer to the Na that has prepared again with 0.24ml ammoniacal liquor
2S
2O
3In the solution, get complex solution A; Take by weighing the 10g Resorcinol, be dissolved in the 8mL deionized water, get solution B.At last A solution is joined in the 14.00mL formaldehyde, transfer in the solution B again, be mixed with argentiferous phenolic aldehyde solution, with this argentiferous phenolic aldehyde solution in 45 ℃ of water-baths preheating about 30 minutes near milk sap the time, splash into continuously above the oil phase post with No. 4.5 syringe needles, when droplet settling forms the canescence gel particle when the oil phase column bottom, it is airtight in the reaction flask that gel particle is packed into, in 85 ℃ of silicone oil baths, wore out 4 days, take out the oil phase in the water flush away gel of back.After the seasoning 5 days, obtaining average diameter of particles is about 1.8mm, globular silver carried organic aerogel of uniform size.Silver carried organic aerogel is placed in the charring furnace, and feeding flow is the N of 800ml/min
2Gas, be warmed up to 600 ℃ with the speed of 5 ℃/min after, kept 3 hours in this temperature, making diameter is about 1.4mm, S
BET=458m
2/ g, of uniform size year silver-colored carbon aerogel particle.
Embodiment 7:R/Ag=30, Ag/NH
3H
2O=0.5, R/F=0.5, R/W=0.9. adopt with example 1 device, are oil phase with the vacuum pump oil, feed hot water heating (going out on advancing down) in sleeve pipe, make the oil phase column temperature keep 65 ℃, and heated constant temperature is started magnetic stirring apparatus at 65 ℃ in the three-necked bottle of below.Get Na
2S
2O
35H
2O2.187g is dissolved in the 3mL deionized water.Take by weighing 0.524g AgNO
3Be dissolved in the 1.5mL deionized water, be made into silver ammino solution, transfer to the Na that has prepared again with 0.22ml ammoniacal liquor
2S
2O
3In the solution, get the silver complex solution A; Take by weighing the 10g Resorcinol, be dissolved in the 7mL deionized water, get solution B.At last A solution is joined in the 12.50mL formaldehyde, transfer to again in the solution B, be mixed with argentiferous phenolic aldehyde solution.With this argentiferous phenolic aldehyde solution in 55 ℃ of water-baths about preheating 4min, when treating that solution becomes near milk sap, mode (pinhole diameter is 0.5mm) with injection splashes into above the oil phase post continuously, when arriving the oil phase column bottom, droplet settling forms the grey gel particle, it is airtight in the reaction flask that gel particle is packed into, in 75 ℃ of constant temperature ovens, wore out 7 days, take out the oil phase in the water flush away gel of back.Directly dried by the fire 24 hours down at 60 ℃, obtaining average diameter of particles is about 1.2mm, silver carried organic aerogel particle of uniform size.Silver carried organic aerogel is placed in the charring furnace, and feeding flow is the N of 800ml/min
2Gas, be warmed up to 1100 ℃ with the speed of 5 ℃/min after, kept 2 hours in this temperature, making diameter is about 0.8mm, of uniform size year silver-colored carbon aerogel particle.
Claims (10)
1. method for preparing silver carried organic aerogel and carbon aerogel particle is with AgNO
3Being mixed with silver complex, is reaction monomers with Resorcinol and formaldehyde, and water as solvent is mixed with argentiferous phenolic aldehyde solution; Each composition proportion is: Resorcinol/Ag=10～100 mass ratioes, and resorcin/formaldehyde=0.4～0.6 mol ratio, the quality of Resorcinol and the volume ratio of water are 0.4～1.5g/ml; When the argentiferous phenolic aldehyde solution for preparing is at room temperature placed or is preheated to solution and becomes near milk sap in 25～55 ℃ of water-baths, adopt the out-phase settling process, above the oil phase post, splash into continuously, oil phase column temperature scope is 65～95 ℃, when droplet settling forms organic gel particle during to the oil phase column bottom, it is airtight in the reaction flask that the organogel particle is packed into, aging down more than 2 days at 75～85 ℃, take out the oil phase in back water or the organic solvent flush away gel particle, seasoning or heating, drying obtain the organic aerogel particle under condition of normal pressure; Afterwards, charing obtains globular silver carried carbon aerogel particle in inert atmosphere.
2. in accordance with the method for claim 1, the coordination agent that it is characterized in that described silver complex is: Na
2S
2O
3/ Na
2SO
3, Ag/Na
2S
2O
3=0.35 mol ratio, Ag/Na
2SO
3=0.5 mol ratio; Perhaps Na
2S
2O
3/ NH
3.H
2O, Ag/Na
2S
2O
3=0.35 mol ratio, Ag/NH
3.H
2O=0.25～0.5 mol ratio.
3. in accordance with the method for claim 1, the oil phase kind that it is characterized in that described oil phase post is that density range is at 0.75～1.0g/cm
3, viscosity is greater than the oils of 0.5mPas.
4. in accordance with the method for claim 3, the oil phase kind that it is characterized in that described oil phase post is vacuum pump oil, silicone oil, peanut oil or whiteruss.
5. according to the described method of one of claim 1-3, it is characterized in that described oil phase post height is 1～3m.
6. according to the described method of one of claim 1-3, it is characterized in that the described argentiferous phenolic aldehyde solution that splashes into continuously is to adopt injection system to splash into above the oil phase post, injecting used pinhole diameter is 0.5～2.5mm.
7. according to the described method of one of claim 1-3, it is characterized in that the used organic solvent of oil phase in the described flush away gel is toluene or acetone.
8. according to the described method of one of claim 1-3, it is characterized in that the described organogel particle aged time is 2～7 days.
9. according to the described method of one of claim 1-3, the temperature that it is characterized in that described organogel particle heating, drying is 60～110 ℃, and the time is 4～24 hours.
10. according to the described method of one of claim 1-3, the temperature that it is characterized in that the charing of described organic aerogel particle is 600～1100 ℃, and carbonization time is 2～3 hours.
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| CN106179408A (en) * | 2016-07-14 | 2016-12-07 | 扬州天辰精细化工有限公司 | A kind of Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material |
| CN107761124A (en) * | 2017-10-23 | 2018-03-06 | 大连理工大学 | A kind of preparation method and application for carrying silver-colored carbon aerogels |
| CN110170322A (en) * | 2019-06-21 | 2019-08-27 | 天津大学 | A kind of preparation method for the platinum/carbon aerogel catalyst loading atom level noble metal |
| CN115084478A (en) * | 2022-07-11 | 2022-09-20 | 成都佰思格科技有限公司 | Hard carbon silver composite negative electrode material, preparation method thereof and lithium ion battery |
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| US2385217A (en) * | 1942-10-09 | 1945-09-18 | Socony Vacuum Oil Co Inc | Gel pellets |
| DE2103243C3 (en) * | 1971-01-25 | 1979-01-11 | Basf Ag, 6700 Ludwigshafen | Process and device for the production of largely spherical, silica-containing hydrogels |
| US5508341A (en) * | 1993-07-08 | 1996-04-16 | Regents Of The University Of California | Organic aerogel microspheres and fabrication method therefor |
| US20040214809A1 (en) * | 2003-04-23 | 2004-10-28 | Biointerface Technologies, Inc. | Stabilized silver-ion sulfite complex compositions and methods |
| CN1281484C (en) * | 2004-05-28 | 2006-10-25 | 中山大学 | Method for preparing carbon gas gel |
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| CN104707662A (en) * | 2015-02-13 | 2015-06-17 | 南京航空航天大学 | Phenolic organic aerogel-doped catalyst and preparation method thereof |
| CN106013640A (en) * | 2016-05-28 | 2016-10-12 | 湖南细心信息科技有限公司 | Air purification wall cloth |
| CN106013640B (en) * | 2016-05-28 | 2018-12-07 | 绍兴艺涵纺织有限公司 | A kind of air purification wall cloth |
| CN106179408A (en) * | 2016-07-14 | 2016-12-07 | 扬州天辰精细化工有限公司 | A kind of Argentous sulfide. load Radix Raphani derives the preparation method of carbon aerogel material |
| CN107761124A (en) * | 2017-10-23 | 2018-03-06 | 大连理工大学 | A kind of preparation method and application for carrying silver-colored carbon aerogels |
| CN107761124B (en) * | 2017-10-23 | 2019-06-07 | 大连理工大学 | A kind of preparation method and application carrying silver-colored carbon aerogels |
| CN110170322A (en) * | 2019-06-21 | 2019-08-27 | 天津大学 | A kind of preparation method for the platinum/carbon aerogel catalyst loading atom level noble metal |
| CN115084478A (en) * | 2022-07-11 | 2022-09-20 | 成都佰思格科技有限公司 | Hard carbon silver composite negative electrode material, preparation method thereof and lithium ion battery |
| CN115084478B (en) * | 2022-07-11 | 2023-03-07 | 成都佰思格科技有限公司 | Hard carbon-silver composite negative electrode material, preparation method thereof and lithium ion battery |
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