CN103691300B - A kind of preparation method of normal-temperature iron desulfurizer - Google Patents
A kind of preparation method of normal-temperature iron desulfurizer Download PDFInfo
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Abstract
The preparation method of normal-temperature iron desulfurizer of the present invention, by adding 0.05 0.5mol/L urea in the mixed solution to soluble cobalt and soluble ferric iron salt, the pH value for adding manganese hydrogen sodium regulating solution is 7.2 7.5；It it is 130 140 DEG C in temperature, pressure precipitates particle to react the FeOOH prepared containing cobalt for 0.5 2 hours under the conditions of 0.12 0.15Mpa；The FeOOH precipitates particle and produces desulfurizing agent product after fluosolids roasting in oxygen-containing atmosphere, under the conditions of 250 300 DEG C.The present inventor has found that the desulfurizing agent that the above method is prepared, compared to desulfurizing agent of the prior art, has higher Sulfur capacity under normal temperature condition by long-term research.
Description
Technical field
The invention belongs to desulfurizing agent field, and in particular to a kind of preparation of the Fe-series desulfurizing agent with high sulfur capacity at normal temperatures
Method.
Background technology
Hydrogen sulfide is widely present in waste gas, natural gas, synthesis gas and the general industry that coal and petroleum chemical industry are produced
It is that one kind has height excitant and corrosive pernicious gas, the hydrogen sulfide of usual very low concentrations in the waste gas of generation
Serious harm is caused to health of human body and nature.Wherein, in the production process of industrial chemicals is produced with coal or oil,
Its produce hydrogen sulfide mainly due in raw material contain more sulphur-containing substance so that the sulphur-containing substance is sent out in process of production
Life is reacted and discharges hydrogen sulfide, and the presence of hydrogen sulfide can directly result in catalyst activity Substance Intoxication in subsequent production workshop section
Inactivation.Therefore, for the harm of removal of hydrogen sulfide, it is necessary to enter the hydrogen sulfide in gas using desulfurizing agent in process of production
Row is removed.
It is used for the desulfurizing agent for removing hydrogen sulfide in the prior art, there is ferriferous oxide desulfurizing agent, Zinc oxide desulfurizer, activated carbon
Desulfurizing agent, many composite oxide of metal desulfurizing agents etc., wherein ferriferous oxide desulfurizing agent is more conventional one kind, such as Chinese patent
Document CN1944273A discloses a kind of ferric oxide desulfurizer, and the preparation method of the desulfurizing agent is：By ferrous sulfate and carbonate
Mixing, is reacted, generation ferrous carbonate and sulfate under conditions of pH value is 8-9；Then after being aoxidized in atmosphere,
Again through washing, filtering, drying iron oxide.
Ferric oxide desulfurizer is one of desulfurizing agent the most traditional, but in terms of desulfurization performance, its desulfurization precision and Sulfur capacity
It is relatively low.In order to improve performance, desulfurizing agent of the prior art generally can also on the basis of above-mentioned Single Iron oxide component
Add other active metal components.Such as China CN1868572A discloses a kind of iron system O composite metallic oxide catalyst, wherein
Aluminum oxide, the 15-45wt% titanium oxide of iron oxide, 15-45wt% containing 20-60wt%, 1-15wt% zinc oxide, 1-15wt% oxygen
Change vanadium.The desulfurizing agent is made using coprecipitation, is 110-160cm2/g than surface, with higher Sulfur capacity.
By those skilled in the art's years of researches, the desulfurization performance of above-mentioned desulfurizing agent in the prior art has significantly
Raising, but still have the disadvantage that：When at normal temperatures in use, the Sulfur capacity of desulfurizing agent is still relatively low in the prior art,
And then the service life and desulfuration efficiency of desulfurizing agent are affected, it is difficult to meet in actual industrial production to desulfuration efficiency
With the requirement of economic performance.
The content of the invention
In order to which the Sulfur capacity for solving desulfurizing agent in the prior art is still relatively low, and then cause service life and the desulfurization of desulfurizing agent
The problem of efficiency is affected, the preparation side of the desulfurizing agent with high sulfur capacity under normal temperature can be obtained the invention provides a kind of
Method.
In order to solve the above-mentioned technical problem, the invention provides a kind of preparation method of normal-temperature iron desulfurizer, including with
Lower step：
（1）Prepare cobalt ions and iron in the mixed aqueous solution of soluble cobalt and soluble ferric iron salt, the mixed aqueous solution
The mol ratio of ion is 1:8-1:15；
（2）The mixed solution is placed in autoclave, 0.05-0.5mol/L urine is added into the mixed solution
Element, the pH value for adding manganese hydrogen sodium regulating solution is 7.2-7.5；
The temperature for controlling the autoclave is 130-140 DEG C, and pressure is 0.12-0.15Mpa, reacts 0.5-2 hours and prepares
Obtain the FeOOH precipitation particle containing cobalt；
（3）The FeOOH containing cobalt is precipitated into particle to be fluidized in oxygen-containing atmosphere, under the conditions of 250-300 DEG C
Roasting；The fluosolids roasting time is 0.5-2 hours；
（4）Particle after fluosolids roasting is mixed with binding agent, pore creating material, after shaping, drying, in 200-250 DEG C of bar
Desulfurizing agent product is obtained after being calcined under part.
The soluble cobalt is Co (NO3) 2, and the soluble ferric iron salt is Fe (NO3) 3 or FeCl3.
The step（1）The mol ratio of middle cobalt ions and iron ion is 1:9-1:11.
The step（2）In, the mixed solution is placed in autoclave, 0.01- is added into the mixed solution
0.2mol/L urea.
The binding agent is the one or two kinds of in bentonite, diatomite.
The pore creating material is wood dust.
The step（4）After particle after roasting is mixed with binding agent, pore creating material, add water and be configured to suspension, pass through
Mist projection granulating is molded.
The step（4）In drying temperature be 90-110 DEG C, drying time be 0.5-2 hours.
The step（4）In time for being calcined under the conditions of 200-250 DEG C be 0.5-2 hours.
The preparation method of normal-temperature iron desulfurizer of the present invention, advantage is：
（1）The preparation method of normal-temperature iron desulfurizer of the present invention, by soluble cobalt and soluble ferric iron salt
Mixed solution in add 0.05-0.5mol/L urea, add manganese hydrogen sodium regulating solution pH value be 7.2-7.5；
Temperature is 130-140 DEG C, and pressure prepares the FeOOH containing cobalt in 0.5-2 hours for reaction under the conditions of 0.12-0.15Mpa
Precipitate particle；The FeOOH precipitates particle and produces desulfurization after fluosolids roasting in oxygen-containing atmosphere, under the conditions of 250-300 DEG C
Agent product.The present inventor passes through long-term research discovery, the desulfurizing agent that the above method is prepared, compared to of the prior art
Desulfurizing agent, has higher Sulfur capacity under normal temperature condition.The reason for causing this phenomenon, the present inventor speculates molten in the mixing
0.05-0.5mol/L urea is added in liquid, the pH value for adding manganese hydrogen sodium regulating solution is 7.2-7.5, and this is conducive to
The FeOOH containing cobalt is generated under follow-up heating, pressurized conditions, and pyrolysis of the sodium acid carbonate in heating process is conducive to
FeOOH particle forms higher specific surface area, the FeOOH surface point of this high-specific surface area in growth course
Rational basic center and cobalt active component are furnished with, the iron oxidation with high desulfurization activity can be further generated after fluosolids roasting
Thing.
（2）The preparation method of normal-temperature iron desulfurizer of the present invention, further limits the step（4）It is middle to be calcined
After particle afterwards is mixed with binding agent, pore creating material, add water and be configured to suspension, be molded through mist projection granulating.Reason is,
The desulfurizing agent that granulating and forming is prepared need to only add a small amount of binding agent and can reach higher intensity, so that with higher sulphur
Hold.
Embodiment
Embodiment 1
The preparation method of desulfurizing agent described in the present embodiment is：
（1）Prepare (the NO containing 0.1mol/LCo3)2With 1.5mol/LFe (NO3)3Mixed aqueous solution, the cobalt ions and iron
The mol ratio of ion is 1:15；
（2）The mixed solution is placed in autoclave, 0.05mol/L urea is added into the mixed solution,
Sodium acid carbonate is slow added into, until the final pH value of solution is 7.2；
The temperature for controlling the autoclave is 130 DEG C, and pressure is 0.12Mpa, and reaction prepares the hydroxyl containing cobalt in 0.5 hour
Base iron oxide precipitates particle；
（3）The FeOOH containing cobalt is precipitated into particle to be fluidized in moving air atmosphere, under the conditions of 250 DEG C
Roasting；The fluosolids roasting time is 0.5 hour；
（4）Particle after fluosolids roasting is mixed with bentonite, sodium carboxymethylcellulose, wherein the bentonitic consumption
For the 5wt% of particle after fluosolids roasting, the consumption of the sodium carboxymethylcellulose is the 3wt% of particle after fluosolids roasting.Through extrusion
Φ is obtained after shaping（5±1）×（10±1）Mm strip, is dried 0.5 hour at 90 DEG C, then is calcined 0.5 hour at 200 DEG C
Obtain desulfurizing agent finished product.
Embodiment 2
The preparation method of desulfurizing agent described in the present embodiment is：
（1）Prepare (the NO containing 0.1mol/LCo3)2And 2.0mol/LFeCl3Mixed aqueous solution, the cobalt ions and iron from
The mol ratio of son is 1:20；
（2）The mixed solution is placed in autoclave, 0.5mol/L urea is added into the mixed solution, then
Sodium acid carbonate is slowly added to, until the final pH value of solution is 7.5；
The temperature for controlling the autoclave is 140 DEG C, and pressure is 0.15Mpa, and reaction prepares the hydroxyl containing cobalt in 2 hours
Iron oxide precipitates particle；
（3）The FeOOH containing cobalt is precipitated into particle in moving air, under the conditions of 300 DEG C and carries out fluidisation roasting
Burn；The fluosolids roasting time is 2 hours；
（4）Particle after fluosolids roasting is mixed with bentonite, sodium carboxymethylcellulose, wherein the bentonitic consumption
For the 5wt% of particle after fluosolids roasting, the consumption of the sodium carboxymethylcellulose is the 3wt% of particle after fluosolids roasting.Through extrusion
Φ is obtained after shaping（5±1）×（10±1）Mm strip, is dried 2 hours, then produced within 2 hours in 250 DEG C of roastings at 110 DEG C
To desulfurizing agent finished product.
Embodiment 3
The preparation method of desulfurizing agent described in the present embodiment is：
（1）Prepare (the NO containing 0.1mol/LCo3)2With 1.6mol/LFe (NO3)3Mixed aqueous solution, the cobalt ions and iron
The mol ratio of ion is 1:16；
（2）The mixed solution is placed in autoclave, 0.01mol/L urea is added into the mixed solution,
Sodium acid carbonate is slow added into, until the final pH value of solution is 7.5；
The temperature for controlling the autoclave is 140 DEG C, and pressure is 0.15Mpa, and reaction prepares the hydroxyl containing cobalt in 2 hours
Iron oxide precipitates particle；
（3）The FeOOH containing cobalt is precipitated into particle in moving air, under the conditions of 300 DEG C and carries out fluidisation roasting
Burn；The fluosolids roasting time is 2 hours；
（4）Particle after fluosolids roasting is mixed with bentonite, sodium carboxymethylcellulose, wherein the bentonitic consumption
For the 5wt% of particle after fluosolids roasting, the consumption of the sodium carboxymethylcellulose is the 3wt% of particle after fluosolids roasting.Through extrusion
Φ is obtained after shaping（5±1）×（10±1）Mm strip, is dried 2 hours, then produced within 2 hours in 250 DEG C of roastings at 110 DEG C
To desulfurizing agent finished product.
Embodiment 4
The preparation method of desulfurizing agent described in the present embodiment is：
（1）Prepare (the NO containing 0.1mol/LCo3)2With 1.8mol/LFe (NO3)3Mixed aqueous solution, the cobalt ions and iron
The mol ratio of ion is 1:18；
（2）The mixed solution is placed in autoclave, 0.2mol/L urea is added into the mixed solution, then
Sodium acid carbonate is slowly added to, until the final pH value of solution is 7.2；
The temperature for controlling the autoclave is 130 DEG C, and pressure is 0.12Mpa, and reaction prepares the hydroxyl containing cobalt in 1 hour
Iron oxide precipitates particle；
（3）The FeOOH containing cobalt is precipitated into particle in air atmosphere, under the conditions of 250 DEG C and carries out fluidisation roasting
Burn；The fluosolids roasting time is 2 hours；
（4）Particle after fluosolids roasting is mixed with bentonite, sodium carboxymethylcellulose, wherein the bentonitic consumption
For the 5wt% of particle after fluosolids roasting, the consumption of the sodium carboxymethylcellulose is the 3wt% of particle after fluosolids roasting.Through extrusion
Φ is obtained after shaping（5±1）×（10±1）Mm strip, is dried 2 hours, then produced within 2 hours in 250 DEG C of roastings at 110 DEG C
To desulfurizing agent finished product.
Embodiment 5
The preparation method of desulfurizing agent described in the present embodiment is：
（1）Prepare (the NO containing 0.1mol/LCo3)2With 1.8mol/LFe (NO3)3Mixed aqueous solution, the cobalt ions and iron
The mol ratio of ion is 1:18；
（2）The mixed solution is placed in autoclave, 0.3mol/L urea is added into the mixed solution, then
Sodium acid carbonate is slowly added to, until the final pH value of solution is 7.2；
The temperature for controlling the autoclave is 130 DEG C, and pressure is 0.12Mpa, and reaction prepares the hydroxyl containing cobalt in 1 hour
Iron oxide precipitates particle；
（3）The FeOOH containing cobalt is precipitated into particle in air atmosphere, under the conditions of 250 DEG C and carries out fluidisation roasting
Burn；The fluosolids roasting time is 2 hours；
（4）Particle after fluosolids roasting is mixed with bentonite, sodium carboxymethylcellulose, wherein the bentonitic consumption
For the 2wt% of particle after fluosolids roasting, the consumption of the sodium carboxymethylcellulose is the 1wt% of particle after fluosolids roasting.Add water
Suspension is configured to, after being molded through mist projection granulating, is dried 2 hours at 110 DEG C, then desulfurizing agent is obtained within 2 hours in 250 DEG C of roastings
Finished product.
In above-described embodiment, step（2）The FeOOH containing cobalt prepared precipitates particle after physical separation
Step is carried out again（3）In fluosolids roasting, the physical separation can be arbitrary solid-liquid separation technique in the prior art, such as from
The heart is separated, is separated by filtration or sedimentation separation.
In addition, step in above-described embodiment 1-5（3）Fluosolids roasting be that particle is placed in fluid bed, it is empty in flowing
Under the drive of gas, particle is suspended among the fluid of motion, is presented " fluidisation state ".In the above embodiment of the present invention 1-5, general
Grain is placed in a diameter of 0.3 ㎡ fluid bed, and the height of stratum granulosum is 10cm, and the flow velocity of the moving air of setting is 0.4m/
s.In fluosolids roasting, the flow velocity of the moving air according to the height of the diameter of fluid bed, stratum granulosum is different and different, this hair
The bright flow velocity for fluosolids roasting has no special restriction, as long as the fluidisation state of particle can be realized, preferably, flow velocity
Scope should be greater than or equal to critical fludization velocity and less than the 105% of critical fludization velocity.
Experimental example
Each 100g of desulfurizing agent for taking above-described embodiment 1 to 5 to prepare, normal temperature (refer to environment temperature, be usually -5 DEG C extremely
45 DEG C) under normal pressure (environmental pressure, usually 1 atmospheric pressure), with containing H2S carries out evaluation test for 40000ppm Standard Gases.Its
In, qualitative detection, can the silver nitrate solution of autogamy 1% to outlet sulphur detect;Quantitative detection, can be integrated micro- using domestic WK-2C
Coulomb meter (Jiangsu Electrical Analysis Instrument Factory's production) is detected that the detection limit of the instrument is 0.2ppm.Testing result is as follows
It is shown.
| Embodiment is numbered | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Sulfur capacity | 63.1% | 62.9% | 65.0% | 66.1% | 69.3% |
Heretofore described desulfurizing agent has high sulfur capacity it can be seen from the above results, up to 63.1%-69.3%.
Comparative example 1
In order to further prove the technique effect for the desulfurizing agent that the present invention is prepared, comparative example, this contrast are also provided with
The preparation method of desulfurizing agent described in example is：
（1）FeOOH particle is prepared using the precipitation method：
By 152 grams of FeSO4It is made into the aqueous solution to be placed in reactor, 58 grams of solid Na is put under agitation2CO3, finally
Mixed aqueous solution pH is adjusted to 8, after reacting 0.5 hour, filtering, filter cake is washed with water, and the filter cake then is made into solid masses
Percentage composition is 30% water slurry, and well is passed through air and aoxidized, until Fe2+/FAlwaysLess than 1%, dried at 100 DEG C, i.e.,
Obtain FeOOH particle；
（2）Using equi-volume process by Co (NO3)2It is immersed on FeOOH particle, wherein Co ions and FeOOH
The mol ratio of middle iron ion is 1:15；
（3）The particle after dipping will be completed and carry out fluosolids roasting in air atmosphere, under the conditions of 250 DEG C；During fluosolids roasting
Between be 0.5 hour；
（4）Particle after roasting is mixed with bentonite, sodium carboxymethylcellulose, Φ is obtained after extruded moulding（5±1）
×（10±1）Mm strip, is dried 0.5 hour at 90 DEG C, then obtains desulfurizing agent finished product within 0.5 hour in 200 DEG C of roastings；Its
Described in bentonitic consumption be the 5wt% of particle after roasting, the consumption of the sodium carboxymethylcellulose is particle after roasting
3wt%。
Above-mentioned desulfurizing agent 100g is taken, is tested under the conditions of described in experimental example, the sulphur of desulfurizing agent in this comparative example is measured
Hold for 41.9%.
Comparative example 2
The preparation method of desulfurizing agent described in this comparative example is：
（1）Prepare (the NO containing 0.1mol/LCo3)2With 1.5mol/LFe (NO3)3Mixed aqueous solution, the cobalt ions and iron
The mol ratio of ion is 1:15；
（2）The mixed solution is placed in autoclave, 0.05mol/L urea is added into the mixed solution,
Sodium acid carbonate is slow added into, until the final pH value of solution is 7.2；
The temperature for controlling the autoclave is 130 DEG C, and pressure is 0.12Mpa, and reaction prepares the hydroxyl containing cobalt in 0.5 hour
Base iron oxide precipitates particle；
（3）The FeOOH precipitation particle containing cobalt is directly calcined in air atmosphere, under the conditions of 250 DEG C
0.5 hour；
（4）Particle after roasting is mixed with bentonite, sodium carboxymethylcellulose, wherein the bentonitic consumption is roasting
The 5wt% of particle after burning, the consumption of the sodium carboxymethylcellulose is the 3wt% of particle after roasting.Φ is obtained after extruded moulding
（5±1）×（10±1）Mm strip, is dried 0.5 hour at 90 DEG C, then obtains desulfurizing agent within 0.5 hour in 200 DEG C of roastings
Finished product.
Compared with Example 1, difference is step to comparative example 2（3）In roasting do not carried out under fluidized state, take
Above-mentioned desulfurizing agent 100g, is tested under the conditions of described in experimental example, and the Sulfur capacity for measuring desulfurizing agent in this comparative example is 52.4%.
From the result of comparative example can be seen that the present invention in the Sulfur capacity of desulfurizing agent for preparing of preparation method it is much big
In comparative example.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Change the protection domain still in the invention.
Claims (9)
1. a kind of preparation method of normal-temperature iron desulfurizer, it is characterised in that comprise the following steps：
(1) cobalt ions and iron ion in the mixed aqueous solution of soluble cobalt and soluble ferric iron salt, the mixed aqueous solution are prepared
Mol ratio be 1:15-1:20；
(2) mixed aqueous solution is placed in autoclave, 0.05-0.5mol/L urine is added into the mixed aqueous solution
Element, is slow added into sodium acid carbonate, until the final pH value of solution is 7.2-7.5；
The temperature for controlling the autoclave is 130-140 DEG C, and pressure is 0.12-0.15Mpa, and reaction is prepared for 0.5-2 hours
FeOOH precipitation particle containing cobalt；
(3) FeOOH containing cobalt is precipitated into particle in oxygen-containing atmosphere, under the conditions of 250-300 DEG C and carries out fluidisation roasting
Burn；The fluosolids roasting time is 0.5-2 hours；
(4) particle after fluosolids roasting is mixed with binding agent, pore creating material, after shaping, drying, under the conditions of 200-250 DEG C
Desulfurizing agent product is obtained after roasting.
2. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that the soluble cobalt is
Co(NO3)2, the soluble ferric iron salt is Fe (NO3)3Or FeCl3。
3. the preparation method of normal-temperature iron desulfurizer according to claim 1 or 2, it is characterised in that in the step (1)
The mol ratio of cobalt ions and iron ion is 1:16-1:18.
4. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that in the step (2), will
The mixed aqueous solution is placed in autoclave, and 0.05-0.2mol/L urea is added into the mixed aqueous solution.
5. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that the binding agent is swelling
One or two kinds of in soil, diatomite.
6. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that the pore creating material is wood chip
Powder.
7. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that the step (4) will roast
After particle after burning is mixed with binding agent, pore creating material, add water and be configured to suspension, be molded through mist projection granulating.
8. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that in the step (4)
Drying temperature is 90-110 DEG C, and drying time is 0.5-2 hours.
9. the preparation method of normal-temperature iron desulfurizer according to claim 1, it is characterised in that in the step (4)
The time being calcined under the conditions of 200-250 DEG C is 0.5-2 hours.
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| CN107082467B (en) * | 2017-03-20 | 2020-10-30 | 中国科学院合肥物质科学研究院 | Iron oxyhydroxide nanorod/foam carbon composite material and preparation method and application thereof |
| CN107497440B (en) * | 2017-08-17 | 2020-05-19 | 江苏天东新材料科技有限公司 | Preparation method and application of multifunctional desulfurizing agent for organic sulfur hydrolysis, absorption and deoxidation |
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