CN104944381B - Method for nano sulfur atomization synthesis - Google Patents
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Abstract
The invention discloses a method for nano sulfur atomization synthesis. The method concretely comprises respectively atomizing a starting material solution and a precipitant solution which are prepared well, controlling gas flow and liquid drop dimension of an atomizer, reacting to synthesize nano sulfur; scattering and precipitating the nano sulfur in a buffer solution and absorbing by-product gas phase through a recycling liquid; filtering the buffer solution through centrifugal separation to obtain nano sulfur sediment products, and performing washing and drying to obtain nano sulfur products; and evaporating and drying the remaining buffer solution and the recycling liquid to obtain reaction by-product chemical sodium salt. Through gas flow atomization, fog drips containing starting materials and fog drips containing a precipitant collide and are mixed with each other, the reaction occurs in the scale range of the fog drips; due to the limitation of the fog drip scale and concentration, the sizes of the products are far smaller than those of the fog drips, and the size uniformity and shape consistency of the obtained products are good. Reacting exhaust gas is fully absorbed through the waste gas recycling liquid and then discharged, and reacting by-products are high-purity sulphurizing salt or sulfite chemical products and are free of environmental pollution.
Description
Technical field
The invention belongs to elemental sulfur chemosynthesis technical field, it is related to a kind of nano-sulfur atomization synthetic method.
Background technology
With Sublimed Sulfur as representative, China produces about 300,000 tons of sulfur every year, and it is in rubber chemicals, daily-use chemical industry, biological medicine
Have a wide range of applications in field, the theoretical research recently as high power capacity, filling power train in vehicle application lithium-sulfur cell soon and application are opened
Send out, further the application market of high purity sulphur is widened and segment, the synthesis of the high purity sulphur of nanoscale and preparation claim
For current lithium-sulfur cell study hotspot field and key technology.
At present, mainly there are distillation-condensation method and solution super-saturation precipitation method with regard to the synthetically prepared of nano-sulfur both at home and abroad
Deng.The former is with Deutsche Bundespatent《Nanoparticles of sulfur obtained by freeze-drying aqueous
sulfur dispersions,useful as an agricultural acaricide or fungicide,and in
lubricants,cosmetics and pharmaceutical compositions》(application number DE19934167, publication date
2001-01-25, publication number DE19934167A1), Chinese patent《High-purity nm sulphur preparing process》(application number
CN03128015, publication date 2003-11-05, publication number CN1453205A) it is representative, it is separated into gas using gasification under sulfur high temperature
Phase atom then passes to the liquid containing dispersant or rapid condensation, obtains the elemental sulfur particle of nanoscale after collection；The latter
Repairing the publishing thesis of equality (preparation of minuteness sulphur powder, Shandong chemical industry, 1999 (6)) with king is representative, using under different temperatures,
Different solubility in specific solvent for the sulfur, separates out the simple substance high purity sulphur particle of preparation nanometer, micro-meter scale by supersaturation.Separately
The nano-sulfur method being seen in outward document report also prepares elemental sulfur particle using wet-chemical sedimentation method preparation liquid phase, mainly fits
Study purposes for laboratory science.Wherein, distillation-condensation method needs pyroprocess, is that a kind of energy consumption is higher, relatively costly
Technical process；Super-saturation precipitation method and the size of sulfur product phase prepared by the wet-chemical sedimentation method, morphological consistency wayward,
The industrial process of inconvenient mass production.
Content of the invention
It is an object of the invention to provide a kind of nano-sulfur is atomized synthetic method, solve existing super-saturation precipitation method and humidifying
The size of high purity sulphur prepared by the sedimentation method, morphological consistency are wayward, the problem of the continuous preparation of inconvenient mass production, simultaneously
Avoid distillation-condensation method high energy consumption, the limitation of high cost.
The technical solution adopted in the present invention is that a kind of nano-sulfur is atomized synthetic method, specifically implements according to the following steps：
Step 1, prepares set out material solution and precipitant solution：
To set out in raw material and precipitant addition solvent, being respectively prepared molar concentration is going out of 0.01mol/L～1mol/L
Send out material solution and precipitant solution；
Step 2, prepares buffer solution and recovered liquid：
Add a small amount of precipitant to adjust pH=5～6 in deionized water, obtain buffer solution；
Add NaOH to adjust pH=10～12 in deionized water, be recycled liquid；
Step 3, atomization synthesis nano-sulfur：
Material solution will be set out and precipitant solution is respectively placed in two nebulizers of reaction unit, the raw material that makes to set out is molten
Liquid and precipitant solution uniform atomizing, atomized drop is synthesized nano-sulfur in the reaction chamber, disperses, sinks in buffer solution
Form sediment；Meanwhile, not completely reaction set out raw material and precipitant in buffer further fully reaction separate out nano-sulfur；Reacted
The by-product gas phase producing in journey is recovered liquid and absorbs；
Step 4, separates product：
Buffer obtained by centrifugation or filtration separation step 3, obtains nano-sulfur precipitated product, and washing, alcohol wash 3～
It is about 7 about, Na to washing liquid pH 5 times+Concentration≤10ppm, then negative pressure drying drying, that is, obtain nano-sulfur product；
Step 5, by-product recovery：
Buffer after being centrifuged or filter through step 4 is evaporated drying, that is, obtains byproduct of reaction chemical products sodium
Salt；Recovered liquid evaporation drying, that is, obtain byproduct of reaction chemical products sodium salt.
The feature of the present invention also resides in,
The molar concentration rate of material solution and the precipitant solution of setting out in step 1 is Na+：H+=1：1～1.2.
The raw material that sets out in step 1 is one or more of sodium sulfide and its hydrate, Sublimed Sulfur or sodium thiosulfate
Mixing.
In step 1 and 2, precipitant is any one in hydrochloric acid, formic acid, acetic acid or sulphuric acid.
In step 1, solvent adopts deionized water or industrial pure water.
In step 3, two nebulizer source of the gas throughputs are 1～10L/min, simultaneously two nebulizer gas in atomization process
Flow is identical, and the size of atomized drop is 1 μm～3 μm.
In step 4, negative pressure drying temperature is 40～100 DEG C, and drying time is 24～48h.
The invention has the beneficial effects as follows, the present invention is by aerodynamic atomization so that containing the droplet of the raw material that sets out and containing heavy
The droplet collisional mixing of shallow lake agent, reacts in the range scale of droplet, is limited by droplet yardstick and concentration, the chi of product
Very little far smaller than droplet sizes, the dimensional homogeneity of products therefrom, morphological consistency are good；Buffer solution is conveyed by fluid-flow pump
Form liquid curtain in reaction chamber and circulate, increase response area and response time and react completely it is ensured that can achieve；Reaction is useless
Gas is discharged after fully being absorbed by waste gas recovery liquid again, and the by-product of reaction is high-purity grade of sulphurizing salt or sulfiting
Chemical product, non-environmental-pollution.
Brief description
Fig. 1 is the structural representation of nano-sulfur particle synthesis reactor of the present invention；
Fig. 2 is nano-sulfur synthetic reaction schematic diagram of the present invention；
Fig. 3 is the nano-sulfur TEM figure that the embodiment of the present invention 2 prepares；
Fig. 4 is single crystal diffraction style figure (a) and EDS energy spectrum diagram (b) of the nano-sulfur that the embodiment of the present invention 2 prepares；
Fig. 5 is the nano-sulfur TEM figure that the embodiment of the present invention 3 prepares.
In figure, 1. exhaust air chamber, 2. recovered liquid feed tube, 3. exhaust chamber, 4. exhaustor, 5. baffle plate b, 6. reclaims chamber, 7.
Reclaim liquid film, 8. recovered liquid, 9. recovered liquid drain pipe, 10. reclaim fluid-flow pump feed tube, 11. buffer drain pipes, 12. bufferings
Fluid-flow pump feed tube, 13. buffer, 14. buffering liquid films, 15. reaction chambers, 16. baffle plate a, 17. precipitant solution nebulizers,
18. set out material solution nebulizer, 19. division boards, 20. buffer feed tubes, 21. recovery fluid-flow pumps, 22. buffering fluid-flow pumps,
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The invention provides a kind of nano-sulfur is atomized synthetic method, specifically implement according to the following steps：
Step 1, prepares set out material solution and precipitant solution：
The raw material that will set out adds in solvent, and prepared molar concentration is set out material solution for 0.01mol/L～1mol/L；To sink
Shallow lake agent adds in solvent, and prepared molar concentration is 0.01mol/L～1mol/L precipitant solution.Wherein set out material solution and sink
The molar concentration rate of shallow lake agent solution is Na+：H+=1：1～1.2.
The raw material that sets out is sodium sulfide and its hydrate (Na2S or Na2S·xH2O), Sublimed Sulfur or sodium thiosulfate
(Na2S2O3) one or more of mixing, precipitant be hydrochloric acid (HCl), formic acid (HCOOH), acetic acid (CH3) or sulfur COOH
Sour (H2SO4) in any one, solvent adopt deionized water or industrial pure water.
Step 2, prepares buffer solution and recovered liquid：
Add a small amount of formic acid, acetic acid, sulphuric acid or hydrochloric acid to adjust pH=5～6 in deionized water, obtain buffer solution.
Add NaOH to adjust pH=10～12 in deionized water, be recycled liquid.
Step 3, atomization synthesis nano-sulfur：
Material solution will be set out and precipitant solution is respectively placed in two nebulizers of reaction unit, control nebulizer gas
Gas reactant flux is 1～10L/min, ensures that two nebulizer throughputs are identical simultaneously, make to set out material solution and precipitant solution equal
Even atomization, the size of atomized drop is 1 μm～3 μm, and atomized drop is synthesized nano-sulfur in the reaction chamber, in buffer solution
Dispersion, precipitation.Meanwhile, not completely reaction set out raw material and precipitant in buffer further fully reaction separate out nanometer
Sulfur.
By-product gas phase H producing in course of reaction2S、SO2Absorbed by the recovered liquid containing NaOH.
Source of the gas adopts industrial nitrogen, compression purify air, plant hydrogen, technical argon etc., and nebulizer adopts adjustable solar term
The high pressure draught atomizing generator of flow.
Step 4, separates product：
Buffer obtained by centrifugation or filtration separation, obtains nano-sulfur precipitated product, and washing, alcohol wash 3～5 times extremely
Washing liquid pH is about 7 about, Na+Concentration≤10ppm, then negative pressure drying dries 24～48h at 40～100 DEG C, that is, obtain nanometer
Sulfur product.
Step 5, by-product recovery：
Buffer after filtering is evaporated drying, that is, obtains byproduct of reaction chemical products sodium salt；Recovered liquid evaporates
It is dried, that is, obtain byproduct of reaction chemical products sodium salt.
The structure of nano-sulfur particle synthesis reactor of the present invention is as shown in figure 1, include being separated by division board 19
Buffer reative cell and recovered liquid reative cell composition, the side wall relative with division board 19 of buffer reative cell is provided with out
Send out material solution nebulizer 18 and precipitant solution nebulizer 17, this side wall is provided with buffer feed tube near reactor top
20, buffer reative cell bottom is provided with buffer drain pipe 11 and buffering fluid-flow pump feed tube 12, buffers fluid-flow pump feed tube
12 are connected with buffer feed tube 20 by pipeline, and pipeline is provided with buffering fluid-flow pump 22；Buffer reaction interior is provided with
Baffle plate a16, baffle plate a16 are located between buffer reactor top and nebulizer place side, are used for making buffer along baffle plate stream
Dynamic, and form buffering liquid film 14；Buffer reactor top is additionally provided with recovered liquid feed tube 2, and recovered liquid feed tube 2 is through isolation
Plate 19 is connected with recovered liquid reative cell；
Recovered liquid reative cell bottom is provided with recovered liquid drain pipe 9 and reclaims fluid-flow pump feed tube 10, reclaims fluid-flow pump and enters
Liquid pipe 10 is connected with recovered liquid feed tube 2 by pipeline, and pipeline is provided with recovery fluid-flow pump 21；The indoor setting of recovered liquid reaction
There is baffle plate b5, baffle plate b5 is located between recovered liquid reactor top and division board 19, is used for making recovered liquid along baffle flows, and shape
Become to reclaim liquid film 14；It is provided with exhaustor 4 on the wall of recovered liquid reative cell side.
Have pore on division board 19, enter recovered liquid reative cell for byproduct of reaction gas phase from buffer reative cell.
The know-why of the present invention is：
Reaction scheme of the present invention is as shown in Fig. 2 using the raw material that sets out (sodium polysulphide or sodium thiosulfate) in precipitant (salt
Acid, formic acid, acetic acid, sulphuric acid etc.) there is metathesis reaction under aqueous environment, separate out the reaction scheme of elemental sulfur：
Na2S1+x+2H+=2Na++xS↓+H2S↑
Or
Na2S2O3+2H+=2Na++S↓+SO2↑+H2O
Control molar concentration Na of set out material solution and precipitant solution+：H+=1：1～1.2；Product Na after reaction+、
H2S、SO2Gas and nano-sulfur are buffered liquid and collect or absorb, and wherein, nano-sulfur suspends or is deposited to buffer is dispersed
Buffer bottom, Na+、H2S、SO2Gas dissolves in buffer, partly undissolved H2S、SO2Gas takes entrance out of with carrier gas
Reclaim chamber, continue to be absorbed as high-purity industrial chemicals Na by the recovery solution containing sodium hydroxide (NaOH)2S or Na2SO3, reaction
Route is shown below：
2NaOH+H2S=Na2S+2H2O
Or
2NaOH+SO2=Na2SO3+H2O
Retain in high-purity nm sulfur in buffer to be dried to obtain using to after the filtration of buffer or centrifugation；Retain
In recovered liquid, byproduct of reaction is dried to obtain using solution concentration and evaporation for high-purity industrial chemicals sodium salt.
In nano-sulfur building-up process, by set out material solution and precipitant solution respectively in the material solution nebulizer that sets out
17 and precipitant solution nebulizer 18 in by aerodynamic atomization, the droplet containing the raw material that sets out and the droplet containing precipitant enter anti-
Answer in chamber 15, collide mixing, reacts in the range scale of droplet, is limited by droplet yardstick and concentration, institute
The size of the nano-sulfur product being formed is far smaller than droplet sizes, and the dimensional homogeneity of products therefrom, morphological consistency are good.
Buffer solution forms buffering liquid film 14 along baffle plate a16 flowing, and buffer reative cell is divided into reaction chamber 15 He
Discarded room 1.Buffer solution is conveyed by buffering fluid-flow pump 22 and forms liquid curtain 14 in reaction chamber and circulate, and increased anti-
Answer area and response time and react completely it is ensured that can achieve.Buffer solution is used for separation product phase and waste gas filters, pH simultaneously<
7 it is ensured that the reaction completely containing the raw material droplet that sets out and nano-sulfur particle separate out.
Reactor off-gas include partly undissolved H2S、SO2Gas and atomization carrier gas, the buffered liquid film of reactor off-gas 14 mistake
After filter, enter exhaust air chamber 1, enter recovered liquid reative cell through the perforate on division board 19.Recovered liquid reative cell is equally by along baffle plate
The recovery liquid film 7 that b5 flowing is formed is divided into recovery chamber 6 and exhaust chamber 3, and the recovered liquid of waste gas enters aerofluxuss after fully absorbing
Room 3, discharges through exhaustor 4.Reclaim solution and convey formation liquid curtain 7 recycle stream in recovery chamber 6 by reclaiming fluid-flow pump 21
Dynamic, increase response area and response time it is ensured that can achieve H2S、SO2Gas fully absorbs.The by-product of reaction is high-purity grade
Sulphurizing salt or sulphite chemical products, non-environmental-pollution.
Embodiment 1
To be set out raw material sodium thiosulfate (Na2S2O3) and hydrochloric acid that precipitant mass fraction is 34%～36% join respectively
Make the aqueous solution that molar concentration is 0.01mol/L, 0.02mol/L, the two molar concentration rate is Na+：H+=1：1.Adjust atomization
The throughput of device is 1L/min.Filling buffer and recovered liquid about 250mL in the reactor, starts and reclaims fluid-flow pump and buffer
Stream pump；Booster air pump makes set out material solution and precipitant solution uniform atomizing, simultaneously monitoring pH of buffer=5～6 and recovery
Liquid pH=12～14, after atomization finishes, buffer obtained by centrifugation, obtain nano-sulfur precipitated product, it is washed,
It is neutrality that alcohol washes 3～5 times to washing liquid, checks Na+Concentration≤10ppm, then negative pressure drying dries 24h at 100 DEG C, that is, obtain non-
Reunion diameter is about 5nm～20nm, pattern is the nano-sulfur product of spherolite shape.
Embodiment 2
The raw material sodium sulfide that will set out is dissolved in water and forms 0.25mol/L aqueous solution, then Na in molar ratio+：S=1：(0.8～
1.5) add Sublimed Sulfur, 4～6h, filtration precipitation are stirred at room temperature, form sodium polysulphide (Na2S1+x) clear solution, quality is divided
The hydrochloric acid deionized water dilution for 34%～36% for the number obtains 0.5mol/L precipitant solution, and the two molar concentration rate is Na+：
H+=1：1.1.The throughput of adjusting atomizer is 5L/min.Fill in the reactor appropriate (liquid level be about 15mm～
25mm) buffer and recovered liquid, starts and reclaims fluid-flow pump and buffering fluid-flow pump；Booster air pump makes set out material solution and precipitant
Solution uniform atomizing, monitoring pH of buffer=5～6 and recovered liquid pH=12～14 simultaneously, after atomization finishes, centrifugation institute
The buffer obtaining, obtains nano-sulfur precipitated product, it is washed, alcohol wash 3～5 times to washing liquid be neutrality, check Na+Concentration≤
10ppm, then negative pressure drying dries 25h at 90 DEG C, that is, obtain that non-agglomerated diameter shown in Fig. 3 is about 30nm～70nm, pattern is
The nano-sulfur product of spherolite shape.Its single crystal diffraction style and EDS energy spectrum diagram are as shown in figure 4, explanation product is the height of highly crystalline
Bright sulfur nanoparticle.
Embodiment 3
The raw material sodium sulfide that will set out is dissolved in water and forms 0.1mol/L aqueous solution, then Na in molar ratio+：S=1：(0.8～
1.5) add Sublimed Sulfur, 4～6h, filtration precipitation are stirred at room temperature, form transparent sodium polysulphide (Na2S1+x, x=0.7～1.4)
Solution, the dilution of formic acid deionized water is obtained 0.2mol/L precipitant solution, and the two molar concentration rate is Na+：H+=1：1.2.
The throughput of adjusting atomizer is 1.5L/min.Filling buffer and recovered liquid about 450mL in the reactor, starts and reclaims liquor stream
Pump and buffering fluid-flow pump；Booster air pump makes set out material solution and precipitant solution uniform atomizing, monitors pH of buffer=5 simultaneously
～6 and recovered liquid pH=12～14, after atomization finishes, buffer obtained by centrifugation, obtain nano-sulfur precipitated product,
It is washed, 3～5, inspection Nas neutral to washing liquid washed by alcohol+Concentration≤10ppm, then negative pressure drying dries 36h at 40 DEG C, that is,
Obtain the about 10nm～30nm of non-agglomerated diameter shown in Fig. 5, pattern is the nano-sulfur product of spherolite shape.
Embodiment 4
To be set out raw material sodium thiosulfate (Na2S2O3) and precipitant acetic acid be configured to respectively molar concentration be 0.5mol/L,
The aqueous solution of 1mol/L, the two molar concentration rate is Na+：H+=1：1.The throughput of adjusting atomizer is about 3L/min.In reaction
Fill appropriate (liquid level is about 15mm～25mm) buffer and recovered liquid in device, start and reclaim fluid-flow pump and buffering liquor stream
Pump；Booster air pump makes set out material solution and precipitant solution uniform atomizing, simultaneously monitoring pH of buffer=5～6 and recovered liquid
PH=12～14, after atomization finishes, buffer obtained by centrifugation, obtain nano-sulfur precipitated product, it is washed, alcohol
Being washed till washing liquid is neutrality, checks Na+Concentration≤10ppm, then negative pressure drying dries 48h at 80 DEG C, that is, obtain non-agglomerated diameter
It is about 100nm～150nm, pattern is the nano-sulfur product of spherolite shape.
Embodiment 5
To be set out raw material sodium thiosulfate (Na2S2O3) and concentrated sulphuric acid that precipitant mass fraction is 98% be configured to respectively
Molar concentration is respectively the aqueous solution of 1mol/L, 1mol/L, and the two molar concentration rate is Na+：H+=1：1.2.Adjusting atomizer
Throughput is 10L/min.Fill appropriate (liquid level is about 15mm～25mm) buffer and recovered liquid in the reactor, start
Reclaim fluid-flow pump and buffering fluid-flow pump；Booster air pump makes set out material solution and precipitant solution uniform atomizing, monitors slow simultaneously
Rush liquid pH=5～6 and recovered liquid pH=12～14, after atomization finishes, buffer obtained by centrifugation, obtain nano-sulfur
Precipitated product, washes to it, alcohol is washed 3～5 times, is neutrality to washing liquid, checks Na+Concentration≤10ppm, then negative pressure is done at 60 DEG C
Dry drying 30h, that is, obtain non-agglomerated diameter about 10nm～50nm, pattern is the nano-sulfur product of spherolite shape.
Claims (4)
1. a kind of nano-sulfur atomization synthetic method is it is characterised in that specifically implement according to the following steps：
Step 1, prepares set out material solution and precipitant solution：
To set out in raw material and precipitant addition solvent, being respectively prepared molar concentration is that setting out of 0.01mol/L～1mol/L is former
Material solution and precipitant solution；
The molar concentration rate of material solution and the precipitant solution of setting out is Na+：H+=1：1～1.2；
The raw material that sets out is the mixing of sodium sulfide and its one of hydrate or sodium thiosulfate or two kinds, or sodium sulfide and its
Hydrate and the reactant of Sublimed Sulfur；
Precipitant is any one in hydrochloric acid, formic acid, acetic acid or sulphuric acid；
Step 2, prepares buffer solution and recovered liquid：
Add a small amount of precipitant to adjust pH=5～6 in deionized water, obtain buffer solution；
Add NaOH to adjust pH=10～12 in deionized water, be recycled liquid；
Step 3, atomization synthesis nano-sulfur：
Material solution will be set out and precipitant solution is respectively placed in two nebulizers of reaction unit, make to set out material solution and
Precipitant solution uniform atomizing, atomized drop is synthesized nano-sulfur in the reaction chamber, dispersion, precipitation in buffer solution；With
When, not completely reaction set out raw material and precipitant in buffer further fully reaction separate out nano-sulfur；In course of reaction
The by-product gas phase producing is recovered liquid and absorbs；
Step 4, separates product：
Buffer obtained by centrifugation or filtration separation step 3, obtains nano-sulfur precipitated product, and washing, alcohol wash 3～5 times
It is 7, Na to washing liquid pH+Concentration≤10ppm, then negative pressure drying drying, that is, obtain nano-sulfur product；
Step 5, by-product recovery：
Buffer after being centrifuged or filter through step 4 is evaporated drying, that is, obtains byproduct of reaction chemical products sodium salt；Return
Receive liquid evaporation drying, that is, obtain byproduct of reaction chemical products sodium salt.
2. a kind of nano-sulfur atomization synthetic method according to claim 1 is it is characterised in that solvent described in step 1 is adopted
Deionized water or industrial pure water.
3. a kind of nano-sulfur atomization synthetic method according to claim 1 is it is characterised in that two mists described in step 3
Change device source of the gas throughput and be 1～10L/min, in atomization process, two nebulizer throughputs are identical, the chi of atomized drop simultaneously
Very little is 1 μm～3 μm.
4. a kind of nano-sulfur atomization synthetic method according to claim 1 is it is characterised in that negative pressure described in step 4 is done
Dry temperature is 40～100 DEG C, and drying time is 24～48h.
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| CN1199850C (en) * | 2003-05-23 | 2005-05-04 | 中国地质大学（武汉） | Prepn process of high-purity nano fulfur |
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