CN104888692B - It is a kind of at the same remove hydrogen sulfide, hydrogen phosphide, the preparation method of arsenic hydride adsorbent - Google Patents
It is a kind of at the same remove hydrogen sulfide, hydrogen phosphide, the preparation method of arsenic hydride adsorbent Download PDFInfo
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Abstract
The present invention discloses a kind of while removing hydrogen sulfide, hydrogen phosphide, the preparation method of arsenic hydride adsorbent, belongs to adsorbent preparation field.The method of the invention is:Wash, dry after diatomite is ground;Dried diatomite is added to after being stirred in HCl solution and stood, then it is neutrality to be washed with distilled water to pH, in drying after filtering;Dried diatomite is added into ultrasonic immersing in metal salt solution, the diatomite after dipping is stood at normal temperatures again, dried, then it is calcined, the diatomite after roasting is put into ultrasonic immersing in acid solution, then the diatomite after dipping is dried into i.e. obtained mesoporous silica-based adsorbent.Preparation method of the present invention is simple to operate, and HCl and metal salt impregnating agent are cheap and easy to get, easily realize industrial applications, also has preferable removal effect at a lower temperature, can be widely used for removing while hydrogen sulfide, hydrogen phosphide and arsenic hydride in all kinds of sources of the gas.
Description
Technical field
The present invention relates to it is a kind of and meanwhile remove hydrogen sulfide, hydrogen phosphide, arsenic hydride adsorbent preparation method, belong to adsorbent
Preparation field.
Background technology
H2S and PH3It is widely present in atmospheric environment, atmospheric environment is discharged into during industrial production and use, can be right
Environment and human body cause serious pollution and harm.H2S is easy to cause catalyst poisoning to inactivate, and has to industrial equipment
Corrosiveness.In addition, dischargeing the H in air without processing2S can form sulfur dioxide, promote photochemical reaction, and finally turn
Sulfate aerosol is turned to, serious environmental problem is brought.AsH is also had in the flue gas that industrial production is discharged3Presence,
AsH3Be at normal temperatures it is a kind of it is colourless, have garlic smell, hypertoxic and fatal gas.Although H2S compares PH3And AsH3It is more easy to remove,
But H2S corrodes production equipment.Very big economic loss is not only brought to industrial production, and adds equipment investment and production
Product cost.While H2S、PH3And AsH3Suction also to human body health exist greatly harm.
Generally, H2S and PH3Removal methods include liquid phase oxidation reducing process, liquid phase catalytic oxidation, absorption process,
Absorption method, wet oxidation process and catalytic decomposition etc..Absorption method is to utilize adsorbent by H2S and PH3It is oxidized to elemental sulfur and five oxygen
Change two phosphorus, the process then removed again.Because S and P2O5Compare H2S and PH3It is easier to be adsorbed by adsorbent.While absorption method
Precision it is high, investment and operating cost are relatively low, there is no power consumption.When unstripped gas sulfur content is relatively low or gas flow compared with
Hour, the effect of absorption method is ideal.AsH3Removing is general also using the method aoxidized, is oxidized as As2O3And H2O。
Absorption method removes H2S、PH3And AsH3Principle be:H2S、PH3And ASH3Turn on the sorbent with active component reaction
It is melted into S, P2O5And As2O3, then these oxidation products be removed in follow-up workshop section.The reaction temperature of absorption is generally below 300
DEG C, and energy consumption is relatively low, and side reaction is less.At the same time, cryogenic absorption H2S、PH3And AsH3Process can avoid raw material gas checking
The generation of the side reactions such as solution, methanation, so the method turns into removing H at present2S、PH3And AsH3One of focus in research field.
Chinese patent CN 103830990A disclose the hair of entitled " a kind of method of hydrogen sulfide in adsorbing and removing methane "
Bright, it is to immerse the material of silica in the solution containing zinc or nitrate that the method, which is related to the preparation method of adsorbent, 100~
After 130 DEG C of drying, it is calcined 2~5 hours at 450~600 DEG C, you can obtain above-mentioned adsorbent.It is characterized in that being repaiied using zinc or copper
The earth silicon material of decorations is sorbing material.The present invention is used as adsorbent, phase based on the earth silicon material that zinc, copper metal are modified
Than traditional carrier, there is obvious advantage in adsorption efficiency, adsorption capacity and use time, therefore, therefore can be with methane
Depriving hydrogen sulphide provides a route efficiently, clean.Chinese patent CN 101564684A disclose entitled " low for purifying
The invention of the transitional metal ion Co modified adsorbent preparation method of concentration hydrogen phosphide ", adsorbing agent carrier involved by this method enters
After row supersound washing, 12~30h of freeze-day with constant temperature under 80~150 DEG C of temperature conditionss is naturally cooling under 0.1MPa vacuums
Room temperature;In dipping modification is carried out to sorbing material with soluble cobalt, 0.5~2h of ultrasonic immersing, cobalt ions containing active component
Molar concentration is 0.1~1mol/L;Adsorbing agent carrier after dipping is cleaned with deionized water, then in 80~150 DEG C of temperature
12~30h of lower drying;Dried carrier is calcined 2~8h at 200~600 DEG C, then drops to room temperature in 0.1MPa.Pass through
Modified adsorbent adsorption, can be achieved waste gas dephosphorization, and have higher adsorption activity within the specific limits.Chinese patent CN
10591553A discloses the invention of entitled " a kind of normal temperature composite desulfurating and dearsenic agent ", can be used for lighter hydrocarbons the present invention relates to one kind
Middle normal temperature desulfurization dearsenification adsorbent, belongs to chemisorbed field of purification.Its preparation method is by mesoporous molecular sieve and active component
Precursor is combined, and selected carrier is silica or sial mesoporous molecular sieve, and active component is copper, iron, manganese, nickel, silver
The nitrate or sulfate of five kinds of elements or the one or more of chloride.Stir and heat after well mixed, after evaporation moisture
Obtain the mixture of active component and carrier.Shaping structures agent is added afterwards to be sufficiently mixed, and is dried after extrusion molding, Ran Hou
0.5~12h is handled at 200~700 DEG C, you can obtain Hydrodearsenic Catalyst.The desulfurating and dearsenic agent prepared using this method has height
Sulfur capacity and arsenic hold, and its desulfurization arsenic-removing rate may be up to more than 99%, and the desulfurating and dearsenic agent can be widely applied to the de- of lighter hydrocarbons
Sulphur dearsenification is pre-processed, and is particularly useful for the desulfurization dearsenification pretreatment of the lighter hydrocarbons containing alkynes.
At present, on adsorbing and removing H simultaneously2S、PH3And AsH3The preparation method of mesoporous silica-based adsorbent have not seen report
Road.
The content of the invention
It is an object of the invention to provide a kind of while the mesoporous silicon substrate of the modification of adsorbing and removing hydrogen sulfide, hydrogen phosphide and arsenic hydride
The preparation method of adsorbent.This method concrete operations are as follows:
(1)Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant,
Dried 3 ~ 7 hours at 100 ~ 150 DEG C;
(2)By step(1)In dried diatomite concentration for 1 ~ 5mol/L HCl solution in stirred at 30~40 DEG C
Mix 0.5 ~ 1.0 hour, then be washed with distilled water to neutrality, dried 3 ~ 7 hours at 100 ~ 150 DEG C after filtering;
(3)By step(2)In dried diatomite be added to ultrasonic immersing 30 ~ 60 minutes in metal salt solution, then will
Diatomite after dipping is dried 3 ~ 7 hours at 100 ~ 150 DEG C, is then calcined 3 ~ 6 hours at 300 ~ 600 DEG C;
(4)By step(3)Diatomite after middle roasting is put into ultrasonic immersing 30 ~ 60 minutes in acid solution, then will dipping
Diatomite afterwards is dried 3 ~ 7 hours at 100 ~ 150 DEG C, that is, mesoporous silica-based adsorbent is made.
Heretofore described diatomite is the mesoporous silica-base material of short distance, with larger specific surface area and higher selectivity
Absorption property.
Step of the present invention(3)Described in metal salt solution be ferric nitrate, copper sulphate, the mixed solution of cobalt nitrate, in metal
The quality of ferric nitrate is the 1 ~ 10% of diatomite quality in salting liquid, and the quality of copper sulphate is the 1 ~ 5% of diatomite quality, cobalt nitrate
Quality be diatomite quality 1 ~ 10%.
Step in the present invention(4)Described in ultrasonic immersing temperature be 20 ~ 50 DEG C, ultrasonic frequency be 28 ~ 40kHz.
Step of the present invention(4)Described in acid solution be HCl, H2SO4、HNO3Or CH3One or more in COOH solution
Mixing, the wherein mass percent of acid solution are 5 ~ 30%.
Beneficial effects of the present invention:
Preparation method of the present invention is simple to operate, and HCl and metal salt impregnating agent are cheap and easy to get, easily realize industrial applications,
Also there is preferable removal effect under lower temperature, the same of hydrogen sulfide in all kinds of sources of the gas, hydrogen phosphide and arsenic hydride is can be widely used for
When remove.
Brief description of the drawings
Fig. 1 is the Cu (NO of load 2%3)2, 1% Co (NO3)3With various concentrations Fe (NO3)3Adsorbent to H2S removal
Effect;
Fig. 2 is the Cu (NO of load 2%3)2, 1% Co (NO3)3With various concentrations Fe (NO3)3Adsorbent to PH3Removal
Effect;
Fig. 3 is the Cu (NO of load 2%3)2, 1% Co (NO3)3With various concentrations Fe (NO3)3Adsorbent to AsH3Go
Except effect.
Embodiment
The description present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings, but the scope of the present invention is not
It is limited to content as described below.
The activity of adsorbent can use H in test following examples2S、PH3And AsH3Clearance represent.
Embodiment 1
Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant, 100
Dried 5 hours in air dry oven at DEG C;By dried diatomite concentration for 1mol/L HCl solution at 30 minutes
Lower stirring dipping 0.5 hour, then to be washed with distilled water to pH constant, dries in air dry oven at 100 DEG C 5 small after filtering
When;Dried diatomite is added into metal salt solution(Constitute ferric nitrate, the nitre of 1% diatomite quality for 2% diatomite quality
The cobalt nitrate of sour copper, 2% diatomite quality)Middle ultrasonic immersing 40 minutes, then by the diatomite after dipping at 100 DEG C in air blast
Dry 5 hours, be then calcined 3 hours at 500 DEG C in drying box;It is 5% that diatomite after roasting is put into mass fraction
Ultrasonic immersing 0.5 hour in HCl solution(The temperature of dipping is 50 DEG C), then by the diatomite after dipping at 100 DEG C in air blast
Dried in drying box 5 hours, that is, mesoporous silica-based adsorbent is made.Fixed bed of the active testing of adsorbent in Φ 4mm × 100mm
Carried out in quartz reactor.Reaction condition is:H2S concentration 139mg/Nm3、PH3Concentration 1112.5mg/Nm3、AsH3Concentration XXmg/
Nm3, relative humidity 49%, air speed 15000h-1, 80 DEG C of reaction temperature, reaction outlet be not detected by H2S, PH3And AsH3.Different iron
Load capacity is to H2S、PH3、AsH3Effect is shown in accompanying drawing, and as seen from the figure when loading 2% ferric nitrate, the adsorbent is to vulcanization
The clearance of hydrogen, hydrogen phosphide and arsenic hydride, which maintains 100%, can respectively reach 120min, 60min, 90min.
Embodiment 2
Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant, at 110 DEG C
Under in air dry oven dry 6 hours;By dried diatomite concentration for 2mol/L HCl solution under 40 minutes
Stirring dipping 0.6 hour, then to be washed with distilled water to pH constant, dries in air dry oven at 110 DEG C 6 small after filtering
When;Dried diatomite is added into metal salt solution(Constitute ferric nitrate, the nitre of 2% diatomite quality for 4% diatomite quality
The cobalt nitrate of sour copper, 4% diatomite quality)Middle ultrasonic immersing 50 minutes, then by the diatomite after dipping at 110 DEG C in air blast
Dry 6 hours, be then calcined 4 hours at 600 DEG C in drying box;It is 15% that diatomite after roasting is put into mass fraction
HNO3Ultrasonic immersing 0.6 hour in solution(The temperature of dipping is 45 DEG C), then by the diatomite after dipping at 110 DEG C in air blast
Dried in drying box 6 hours, that is, mesoporous silica-based adsorbent is made.Fixed bed of the active testing of adsorbent in Φ 4mm × 100mm
Carried out in quartz reactor.Reaction condition is:H2S concentration 139mg/Nm3、PH3Concentration 1112.5mg/Nm3、AsH3Concentration XXmg/
Nm3, relative humidity 49%, air speed 15000h-1, 80 DEG C of reaction temperature, reaction outlet be not detected by H2S, PH3And AsH3.Different iron
Load capacity is to H2S、PH3、AsH3Effect sees accompanying drawing, and as seen from the figure when loading 4% ferric nitrate, the adsorbent is to vulcanization
The clearance of hydrogen, hydrogen phosphide and arsenic hydride, which maintains 100%, can respectively reach 60min, 30min, 120min.
Embodiment 3
Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant, at 120 DEG C
Under in air dry oven dry 7 hours;By dried diatomite concentration for 3mol/L HCl solution under 50 minutes
Stirring dipping 0.7 hour, then to be washed with distilled water to pH constant, dries in air dry oven at 120 DEG C 7 small after filtering
When;Dried diatomite is added into metal salt solution(Constitute ferric nitrate, the nitre of 3% diatomite quality for 6% diatomite quality
The cobalt nitrate of sour copper, 6% diatomite quality)Middle ultrasonic immersing 60 minutes, then by the diatomite after dipping at 120 DEG C in air blast
Dry 7 hours, be then calcined 4.5 hours at 450 DEG C in drying box;It is 20% that diatomite after roasting is put into mass fraction
H2SO4Ultrasonic immersing 0.7 hour in solution(The temperature of dipping is 40 DEG C), then by the diatomite after dipping at 120 DEG C in drum
Dried in wind drying box 7 hours, that is, mesoporous silica-based adsorbent is made.Fixation of the active testing of adsorbent in Φ 4mm × 100mm
Carried out in bed quartz reactor.Reaction condition is:H2S concentration 139mg/Nm3、PH3Concentration 1112.5mg/Nm3、AsH3Concentration
XXmg/Nm3, relative humidity 49%, air speed 15000h-1, 80 DEG C of reaction temperature, reaction outlet be not detected by H2S, PH3And AsH3.No
With iron load capacity to H2S、PH3、AsH3Effect is shown in accompanying drawing, and as seen from the figure when loading 6% ferric nitrate, the adsorbent is to sulphur
Change hydrogen, hydrogen phosphide and arsenic hydride clean-up effect preferably, its clearance maintain 100% can respectively reach 150min, 240min,
210min。
Embodiment 4
Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant, at 130 DEG C
Under in air dry oven dry 4 hours;By dried diatomite concentration for 4mol/L HCl solution under 60 minutes
Stirring dipping 0.8 hour, then to be washed with distilled water to pH constant, dries in air dry oven at 130 DEG C 4 small after filtering
When;Dried diatomite is added into metal salt solution(Constitute ferric nitrate, the nitre of 4% diatomite quality for 8% diatomite quality
The cobalt nitrate of sour copper, 8% diatomite quality)Middle ultrasonic immersing 45 minutes, then by the diatomite after dipping at 130 DEG C in air blast
Dry 4 hours, be then calcined 5 hours at 500 DEG C in drying box;It is 25% that diatomite after roasting is put into mass fraction
CH3Ultrasonic immersing 0.8 hour in COOH solution(The temperature of dipping is 30 DEG C), then by the diatomite after dipping at 130 DEG C in
Dried in air dry oven 4 hours, that is, mesoporous silica-based adsorbent is made;The active testing of adsorbent is consolidated Φ 4mm × 100mm's
Carried out in fixed bed quartz reactor;Reaction condition is:H2S concentration 139mg/Nm3、PH3Concentration 1112.5mg/Nm3、AsH3Concentration
XXmg/Nm3, relative humidity 49%, air speed 15000h-1, 80 DEG C of reaction temperature, reaction outlet be not detected by H2S, PH3And AsH3;No
With iron load capacity to H2S、PH3、AsH3Effect is shown in accompanying drawing, and as seen from the figure when loading 8% ferric nitrate, the adsorbent is to sulphur
The clearance of change hydrogen, hydrogen phosphide and arsenic hydride, which maintains 100%, can respectively reach 90min, 180min, 180min.
Embodiment 5
Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant, at 150 DEG C
Under in air dry oven dry 3 hours;By dried diatomite concentration for 5mol/L HCl solution under 90 minutes
Stirring dipping 1.0 hours, then to be washed with distilled water to pH constant, dries in air dry oven at 150 DEG C 3 small after filtering
When;Dried diatomite is added into metal salt solution(Constitute ferric nitrate for 10% diatomite quality, 5% diatomite quality
The cobalt nitrate of copper nitrate, 10% diatomite quality)Middle ultrasonic immersing 30 minutes, then by the diatomite after dipping at 150 DEG C in drum
Dry 3 hours, be then calcined 6 hours at 600 DEG C in wind drying box;It is 30% that diatomite after roasting is put into mass fraction
HCl solution in ultrasonic immersing 1.0 hours(The temperature of dipping is 20 DEG C), then by the diatomite after dipping at 150 DEG C in drum
Dried in wind drying box 3 hours, that is, mesoporous silica-based adsorbent is made.Fixation of the active testing of adsorbent in Φ 4mm × 100mm
Carried out in bed quartz reactor.Reaction condition is:H2S concentration 139mg/Nm3、PH3Concentration 1112.5mg/Nm3、AsH3Concentration
XXmg/Nm3, relative humidity 49%, air speed 15000h-1, 80 DEG C of reaction temperature, reaction outlet be not detected by H2S, PH3And AsH3.No
With iron load capacity to H2S、PH3、AsH3Effect is shown in accompanying drawing, as seen from the figure when loading 10% ferric nitrate, the adsorbent pair
The clearance of hydrogen sulfide, hydrogen phosphide and arsenic hydride, which maintains 100%, can respectively reach 60min, 150min, 150min.
Claims (1)
1. it is a kind of at the same remove hydrogen sulfide, hydrogen phosphide, the preparation method of arsenic hydride adsorbent, it is characterised in that specifically include with
Lower step:
(1)Diatomite is ground and 40 ~ 60 mesh are sieved into, 4 ~ 6 times is then washed and is suspended without muddy thing to supernatant, 100 ~
Dried 4 ~ 7 hours at 150 DEG C;
(2)By step(1)In dried diatomite concentration for 1 ~ 5mol/L HCl solution at 30~40 DEG C stir
0.5 ~ 1.0 hour, then neutrality is washed with distilled water to, dried 4 ~ 7 hours at 100 ~ 150 DEG C after filtering;
(3)By step(2)In dried diatomite be added to ultrasonic immersing 30 ~ 60 minutes in metal salt solution, then will dipping
Diatomite afterwards is dried 4 ~ 7 hours at 100 ~ 150 DEG C, is then calcined 3 ~ 6 hours at 300 ~ 600 DEG C;
(4)By step(3)Diatomite after middle roasting is put into ultrasonic immersing 30 ~ 60 minutes in acid solution, then by after dipping
Diatomite is dried 4 ~ 7 hours at 100 ~ 150 DEG C, that is, mesoporous silica-based adsorbent is made;
Step(3)Described in metal salt solution be ferric nitrate, copper sulphate, the mixed solution of cobalt nitrate, the nitre in metal salt solution
The quality of sour iron is the 1 ~ 10% of diatomite quality, and the quality of copper sulphate is the 1 ~ 5% of diatomite quality, and the quality of cobalt nitrate is silicon
The 1 ~ 10% of diatomaceous earth quality;
Step(4)Described in ultrasonic immersing temperature be 20 ~ 50 DEG C, ultrasonic frequency be 28 ~ 40KHz;
Step(4)Described in acid solution be HCl, H2SO4、HNO3Or CH3One or more mixing in COOH solution, wherein acid
Property solution mass percent be 5 ~ 30%.
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CN106693881B (en) * | 2016-11-21 | 2019-07-05 | 昆明理工大学 | A kind of modified mesopore oxide adsorbent of acid and the preparation method and application thereof |
CN109675428A (en) * | 2018-12-21 | 2019-04-26 | 昆明理工大学 | A kind of SiO2The preparation method and applications of@CuO Core-shell structure material |
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