CN112604491A - Nano desulfurizer, preparation method and reaction system - Google Patents

Nano desulfurizer, preparation method and reaction system Download PDF

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CN112604491A
CN112604491A CN202011594178.5A CN202011594178A CN112604491A CN 112604491 A CN112604491 A CN 112604491A CN 202011594178 A CN202011594178 A CN 202011594178A CN 112604491 A CN112604491 A CN 112604491A
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desulfurizer
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陶凌云
孙睿雷
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Hubei Junran New Material Co ltd
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/81Solid phase processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/48Sulfur compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus

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Abstract

The invention provides a nano desulfurizer, a preparation method and a system, wherein the nano desulfurizer comprises nano Al2O3Nano ZnO and nano CuO, and nano Al2O3The molar ratio of the nano ZnO to the nano CuO is as follows: (0.8-1.5): (0.8-1.5): (1.8-2.5). Compared with the prior art, the invention has the beneficial effects that: the desulfurizer of the invention adopts a rotary liquid film reactor to carry out coprecipitation reaction, and nano Al with the sulfur capacity of more than 15 percent is obtained after hydrothermal crystallization reaction2O3The desulfurizing agent of three nano oxide systems of nano ZnO and nano CuO has greatly improved desulfurizing activity and sulfur capacity.

Description

Nano desulfurizer, preparation method and reaction system
Technical Field
The invention belongs to the field of desulfurizer preparation, and particularly relates to a nano desulfurizer, a preparation method and a reaction system.
Background
With the development of gas purification technology, the traditional fine desulfurization technology can not meet the industrial requirements, and the current large-scale methanol synthesis device requires that the total sulfur inlet is less than 0.01 x 10-6(v/v), the traditional desulfurizing agents such as zinc oxide, iron oxide and the like are difficult to meet the requirements. Multicomponent metal oxide systems are now generally used(e.g., copper oxide-zinc oxide-iron oxide) to meet specifications.
The existing multi-component metal oxide system is prepared in a kettle type reactor by adopting a coprecipitation method, the production is intermittent, the preparation time is prolonged, the production efficiency is low, the product quality is influenced by factors such as stirring speed, material concentration, reaction temperature and the like, and the sulfur capacity of the obtained desulfurizer is low.
Disclosure of Invention
In order to solve the technical problems, the invention provides a nano desulfurizer, a preparation method and a reaction system.
The specific technical scheme is as follows:
the nanometer desulfurizing agent is characterized by comprising nanometer Al2O3, nanometer ZnO and nanometer CuO, wherein the nanometer Al is selected from the group consisting of2O3The molar ratio of the nano ZnO to the nano CuO is as follows: (0.8-1.5): (0.8-1.5): (1.8-2.5);
the preparation method of the nano desulfurizer comprises the following steps:
the difference between the preparation method of the nano desulfurizer and the preparation method thereof is that the preparation method of the nano desulfurizer comprises the following steps:
step S1: mixing the mixed ionic solution and a precipitator in a rotary liquid membrane reactor under high-speed shearing and carrying out coprecipitation reaction to obtain a coprecipitation reactant;
step S2: carrying out hydrothermal crystallization reaction on the coprecipitation reactant, and removing impurities to obtain a first precipitate;
step S3: forming the first precipitate, and drying to obtain a precursor;
step S4: roasting the precursor to obtain the nano desulfurizer;
wherein the mixed ion solution comprises Al3+,Zn2+And Cu2+Said Al3+,Zn2+And Cu2+The molar ratio of (1.6-3): (0.8-1.5): (1.8-2.5).
Compared with the prior art, the invention has the beneficial effects that: the desulfurizer of the invention adopts rotationThe liquid film reactor carries out coprecipitation reaction, and nano Al with the sulfur capacity of more than 15 percent is obtained after hydrothermal crystallization reaction2O3The desulfurizing agent of three nano oxide systems of nano ZnO and nano CuO has greatly improved desulfurizing activity and sulfur capacity.
Further, the nano Al2O3The molar ratio of the nano ZnO to the nano CuO is as follows: 1: 1: 2.
the difference between the preparation method of the nano desulfurizer and the preparation method thereof is that the preparation method of the nano desulfurizer comprises the following steps:
step S1: mixing the mixed ionic solution and a precipitator in a rotary liquid membrane reactor under high-speed shearing and carrying out coprecipitation reaction to obtain a coprecipitation reactant;
step S2: carrying out hydrothermal crystallization reaction on the coprecipitation reactant, and removing impurities to obtain a first precipitate;
step S3: forming the first precipitate, and drying to obtain a precursor;
step S4: roasting the precursor to obtain the nano desulfurizer;
wherein the mixed ion solution comprises Al3+,Zn2+And Cu2+Said Al3+,Zn2+And Cu2+The molar ratio of (1.6-3): (0.8-1.5): (1.8-2.5).
Further, the mixed ion solution includes Al3+,Zn2+And Cu2+Said Al3+,Zn2+And Cu2+In a molar ratio of 2: 1: 2.
further, in the step S1, the precipitating agent is K2CO3Solution and/or Na2CO3A solution; wherein CO in the precipitant3 2-The metal ions in the mixed ion solution can be completely precipitated.
Furthermore, the clearance between a rotor and a stator of the rotary liquid film reactor is 10-30 μm, the shearing rate is 2000-5000 rpm, the reaction temperature is 30-60 ℃, and the material flow rate is 100-150 kg/h.
Further, in the step S2, the crystallization temperature is 100 to 180 ℃, and the crystallization time is 10 to 60 min.
Further, step S3: and after the filter cake is washed, adding a binder, uniformly mixing, extruding into strips, drying the formed desulfurizer in the shade, and drying to obtain a precursor.
Further, in the step S4, the precursor is roasted at 350-550 ℃ for 2-5 h to obtain the nano desulfurizer.
Further, in the step S1, Al3+Has a concentration of 1.0mol/L, Zn2+Has a concentration of 0.5mol/L, Cu2+Has a concentration of 1.0mol/L, CO3 2-The concentration of (2) is 1.5 mol/L.
In the step S1, the clearance between a rotor and a stator of the rotary liquid film reactor is 10-20 μm, the shearing rate is 3000 rpm-5000 rpm, the reaction temperature is 40-50 ℃, and the material flow rate is 100 kg/h-150 kg/h;
in the step S2, the crystallization temperature is 140-150 ℃, and the crystallization time is 20-35 min;
in the step S4, the precursor is roasted for 4 to 5 hours at the temperature of 400 to 500 ℃ to obtain the nano desulfurizer.
The beneficial effect of adopting the further technical scheme is that: the control parameter is in the range, and the desulfurization capacity can be improved to more than 20%.
The reaction system for preparing the nano desulfurizer is characterized by comprising a rotary liquid film reactor and a tubular crystallization reactor which are sequentially connected, wherein the rotary liquid film reactor is used for mixing a mixed ionic solution and a precipitator under high-speed shearing and carrying out coprecipitation reaction, and the tubular crystallization reactor is used for carrying out hydrothermal crystallization reaction on a coprecipitation reactant.
Compared with the prior art, the invention has the beneficial effects that:
(1) the rotary liquid film reactor and the tubular hydrothermal crystallizer are adopted to overcome the defect of batch reaction of the kettle type reactor, and the production efficiency is improved by continuous feeding reaction;
(2) the high-speed shearing movement of the rotary liquid film reactor enables the metal salt and the precipitator to be quickly mixed and react to form a large number of tiny crystal nuclei instantly, and the crystal nuclei are generated into nano particles after crystallization treatment, so that the rotary liquid film reactor has good desulfurization activity and sulfur capacity.
(3) Compared with a kettle type reactor, the tubular crystallization reactor can quickly finish the crystallization reaction of the product under the action of hydrothermal at higher temperature, and simultaneously, the tubular crystallization reactor is combined with a liquid membrane reactor to ensure that the generation process is continuously carried out.
Further, the liquid membrane reactor comprises:
the static disc is provided with a feeding hole;
the movable disc is arranged outside the static disc, an adjustable gap is formed between the movable disc and the static disc, and the movable disc can rotate relative to the static disc;
the closed disc is arranged on the opposite side of the movable disc, a gap opening between the movable disc and the static disc is closed, and a discharge hole is formed in the gap opening of the closed disc;
and
the feeding pipe is connected with the feeding hole and comprises a first feeding pipe and a second feeding pipe which are embedded inside and outside;
wherein the adjustable gap is in the range of 5-200 μm.
Further, the movable disc comprises an upper plate and a side plate which are movably connected, and the upper plate and the side plate are both provided with slit adjusting bolts;
further, the movable disc is connected with a speed-adjustable motor.
The beneficial effect of adopting the further technical scheme is that: rotatory liquid membrane reactor comprises quiet dish and movable disk, and reaction material gets into respectively the feeding with the sediment, then reacts in clearance department, and the metal salt solution walks the movable disk and drives high-speed rotation by the motor, and the material forms the liquid film in movable disk and fixed disk clearance, is dragged high-speed the mixing by shear stress, can form the crystal nucleus rapidly.
Drawings
FIG. 1 is a system diagram of example 1;
FIG. 2 is a cross-sectional view of a rotating liquid membrane reactor;
FIG. 3 is a schematic diagram of a desulfurizing agent preparation process;
1-rotating liquid film reactor, 2-tubular crystallization reactor, 101-static disc, 102-movable disc, 1021-upper plate, 1022-side plate, 1023-slit adjusting bolt, 103-adjustable gap, 104-second feeding pipe, 105-first feeding pipe, 106-speed adjustable motor, 107-closed disc and 1071-discharge hole.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1 reaction System for preparing Nano desulfurizing agent
As shown in fig. 1, includes: the device comprises a rotary liquid film reactor 1 and a tubular crystallization reactor 2 which are connected in sequence, wherein the rotary liquid film reactor 1 is used for mixing a mixed ionic solution and a precipitator under high-speed shearing and carrying out coprecipitation reaction, and the tubular crystallization reactor is used for carrying out hydrothermal crystallization reaction on a coprecipitation reactant.
As shown in fig. 2, the rotary liquid membrane reactor 1 includes:
a stationary disc 101, wherein the stationary disc 101 is provided with a feeding hole (not shown in the figure);
a movable disc 102 arranged outside the fixed disc 101, wherein an adjustable gap 103 exists between the movable disc 102 and the fixed disc 101, and the movable disc 102 can rotate relative to the fixed disc 101;
the closing disc 107 is arranged on the opposite side of the movable disc 102, a gap between the movable disc 102 and the static disc 101 is closed, and a discharge hole 1071 is formed in the gap of the closing disc 107;
and
and the feeding pipe is connected with the feeding hole and comprises a first feeding pipe 105 and a second feeding pipe 104 which are embedded in an inner sleeve mode, in the embodiment, the mixed metal solution enters from the second feeding pipe 104, and the precipitating agent enters from the first feeding pipe 105.
Wherein the adjustable gap is in the range of 5-200 μm.
In this embodiment, the movable plate includes an upper plate 1021 and a side plate 1022 which are movably connected, the upper plate and the side plate are both provided with a slit adjusting bolt 1023, and the distance of the gap is adjusted by adjusting the slit adjusting bolt 1023.
The rotating disk 102 is connected to an adjustable speed motor 106, which controls the rotating disk to rotate at different speeds.
Example 2
The nano-desulfurizer is prepared by the following method
Preparing metal salt solution Al (NO)3)3、Zn(NO3)2And Cu (NO)3)2Mixing the solution with Al in the solution3+1.0mol/L、Zn2 +0.5mol/L、Cu2+1.0mol/L, and preparing 1.5mol/L sodium carbonate solution as a precipitator.
Step S1: and (2) pumping the precipitant and a metal salt solution into a liquid film reactor by using a metering pump, finely adjusting the feeding amount of the precipitant to maintain the reaction liquid to be alkalescent, wherein the ph is 8-9, the gap between a rotor and a stator of the liquid film reactor is 10 mu m, the shearing rate is 5000rpm, the reaction temperature is 40 ℃, and the material flow rate is 100 kg/h.
Step S2: pumping the reaction liquid into a tubular crystallization reactor at the outlet of the liquid film reactor by a pump, controlling the crystallization temperature at 135 ℃, completing the crystallization reaction for 20min, carrying out solid-liquid separation, and washing the separated solid by pure water to remove metal ions and nitrate radicals remained in the filter cake.
Step S3: and after the filter cake is washed, adding a binder, uniformly mixing, extruding into strips, drying the formed desulfurizer in the shade for 20 hours, and drying at 140 ℃ for 4 hours to obtain a precursor.
Step S4: and roasting the dried desulfurizer at 450 ℃ for 3h to obtain a deep desulfurizer finished product.
Example 3
The nano-desulfurizer is prepared by the following method
Preparing metal salt solution Al (NO)3)3、Zn(NO3)2And Cu (NO)3)2Mixing the solution with Al in the solution3+1.0mol/L、Zn2 +0.5mol/L、Cu2+1.0mol/L, preparation 1.5mol/L sodium carbonate solution is used as a precipitator.
Step S1: and (2) pumping the precipitant and a metal salt solution into a liquid film reactor by using a metering pump, finely adjusting the feeding amount of the precipitant to maintain the reaction liquid to be alkalescent, wherein the ph is 8-9, the gap between a rotor and a stator of the liquid film reactor is 10 mu m, the shearing rate is 5000rpm, the reaction temperature is 50 ℃, and the material flow rate is 120 kg/h.
Step S2: pumping the reaction liquid into a tubular crystallization reactor at the outlet of the liquid film reactor by a pump, controlling the crystallization temperature at 150 ℃, completing the crystallization reaction for 25min, carrying out solid-liquid separation, and washing the separated solid by pure water to remove metal ions and nitrate radicals remained in the filter cake.
Step S3: and after the filter cake is washed, adding a binder, uniformly mixing, extruding into strips, drying the formed desulfurizer in the shade for 20 hours, and drying at 140 ℃ for 4 hours to obtain a precursor.
Step S4: and roasting the dried desulfurizer at 500 ℃ for 2.5h to obtain a deep desulfurizer finished product.
Example 4
The nano-desulfurizer is prepared by the following method
Preparing metal salt solution Al (NO)3)3、Zn(NO3)2And Cu (NO)3)2Mixing the solution with Al in the solution3+1.0mol/L、Zn2 +0.5mol/L、Cu2+1.0mol/L, and preparing 1.5mol/L sodium carbonate solution as a precipitator.
Step S1: and (2) pumping the precipitant and a metal salt solution into a liquid membrane reactor by using a metering pump, finely adjusting the feeding amount of the precipitant to maintain the reaction liquid to be alkalescent, wherein ph is about 8-9, the clearance between a rotor and a stator of the liquid membrane reactor is 20 mu m, the shearing rate is 3000rpm, the reaction temperature is 40 ℃, and the material flow rate is 150 kg/h.
Step S2: pumping the reaction liquid into a tubular crystallization reactor at the outlet of the liquid film reactor by a pump, controlling the crystallization temperature at 130 ℃, completing the crystallization reaction for 35min, carrying out solid-liquid separation, and washing the separated solid by pure water to remove metal ions and nitrate radicals remained in the filter cake.
Step S3: and after the filter cake is washed, adding a binder, uniformly mixing, extruding into strips, drying the formed desulfurizer in the shade for 15 hours, and drying at 135 ℃ for 3 hours to obtain a precursor.
Step S4: and roasting the dried desulfurizer at 400 ℃ for 5h to obtain a deep desulfurizer finished product.
Example 5
The nano-desulfurizer is prepared by the following method
The gap between the rotor and the stator of the rotary liquid membrane reactor was 30 μm compared to example 2.
Example 6
The nano-desulfurizer is prepared by the following method
The shear rate of the rotary liquid membrane reactor was 2000rpm compared to example 2.
Example 7
The nano-desulfurizer is prepared by the following method
Compared with the example 3, in the step S2, the crystallization temperature is 100 ℃, and the crystallization time is 60 min.
Example 8
The nano-desulfurizer is prepared by the following method
Compared with the example 3, in the step S2, the crystallization temperature is 180 ℃ and the crystallization time is 10 min.
Example 9
The nano-desulfurizer is prepared by the following method
Compared with the embodiment 4, the precursor is roasted for 5 hours at 350 ℃ to obtain the nano desulfurizer.
Example 10
The nano-desulfurizer is prepared by the following method
Compared with the embodiment 4, the precursor is roasted for 2h at 550 ℃ to obtain the nano desulfurizer.
Comparative example 1
The desulfurizing agent was prepared by the following method
Preparing metal salt solution Al (NO)3)3、Zn(NO3)2And Cu (NO)3)2Mixing the solution with Al in the solution3+1.0mol/L、Zn2 +0.5mol/L、Cu2+1.0mol/L, and preparing 1.5mol/L sodium carbonate solution as a precipitator.
Step S1: mixing a precipitator and a metal salt solution into a reactor, finely adjusting the feeding amount of the precipitator to maintain the reaction solution to be alkalescent, controlling ph to be about 8-9, reacting under stirring at the reaction temperature of 40 ℃ for 3 hours, carrying out solid-liquid separation after the reaction is finished, and washing the separated solid with pure water to remove metal ions and nitrate radicals remained in a filter cake.
Step S2: and after the filter cake is washed, adding a binder, uniformly mixing, extruding into strips, drying the formed desulfurizer in the shade for 20 hours, and drying at 140 ℃ for 4 hours to obtain a precursor.
Step S3: and roasting the dried desulfurizer at 450 ℃ for 3h to obtain a deep desulfurizer finished product.
Comparative example 2
The nano-desulfurizer is prepared by the following method
Preparing metal salt solution Fe (NO)3)3、Zn(NO3)2And Cu (NO)3)2Mixing the solution, Fe in the solution3+1.0mol/L、Zn2 +0.5mol/L、Cu2+1.0mol/L, and preparing 1.5mol/L sodium carbonate solution as a precipitator.
Step S1: and (2) injecting a precipitator and a metal salt solution into the liquid membrane reactor by using a metering pump, finely adjusting the feeding amount of the precipitator to maintain the reaction liquid to be alkalescent, controlling the ph to be about 8-9, controlling the clearance between a rotor and a stator of the liquid membrane reactor to be 10 mu m, controlling the shear rate to be 5000rpm, controlling the reaction temperature to be 40 ℃ and controlling the material flow rate to be 100 kg/h.
Step S2: pumping the reaction liquid into a tubular crystallization reactor at the outlet of the liquid film reactor by a pump, controlling the crystallization temperature at 135 ℃, completing the crystallization reaction for 20min, carrying out solid-liquid separation, and washing the separated solid by pure water to remove metal ions and nitrate radicals remained in the filter cake.
Step S3: and after the filter cake is washed, adding a binder, uniformly mixing, extruding into strips, drying the formed desulfurizer in the shade for 20 hours, and drying at 140 ℃ for 4 hours to obtain a precursor.
Step S4: and roasting the dried desulfurizer at 450 ℃ for 3h to obtain a deep desulfurizer finished product.
Example 11
Desulfurization Activity and Sulfur Capacity test experiments
The operation steps are as follows:
1) preparing a desulfurization reaction gas with the concentration of hydrogen sulfide of-500 mg/L by using nitrogen as a balance gas, standing the reaction gas for 24 hours after the reaction gas is prepared, and analyzing and calibrating the concentration c (mg/L) of the hydrogen sulfide.
2) Taking 30ml of desulfurizer, weighing and recording the weight m, loading the desulfurizer into a reaction tube, connecting a gas path, introducing nitrogen, and heating the reactor to 180-200 ℃.
3) After the reaction temperature is stable, cutting in desulfurization reaction gas, closing the temperature-rising nitrogen, adjusting the flow of the reaction gas, and controlling the space velocity SV at 200-500 h-1Left and right, reaction start time t1 is recorded.
4) The reaction outlet gas was taken every 0.5 hour for analysis, and when the outlet hydrogen sulfide concentration exceeded 0.01ppm, the reaction was stopped, and the reaction stop time t2 was recorded.
5) According to the formula of hydrogen sulfide sulfur capacity
Figure BDA0002869451800000101
And calculating the sulfur capacity of the desulfurizer.
The test results are shown in table 1.
TABLE 1 Sulfur capacity test results
Sample (I) Sulfur content (%)
Example 2 26
Example 3 22
Example 4 24
Example 5 16
Example 6 19
Example 7 19
Example 8 17
Example 9 15
Example 10 16
Comparative example 1 7
Comparative example 2 10
As can be seen from table 1, in the example of the present invention, compared to comparative example 1, the sulfur capacity of the co-precipitation reaction in the rotary liquid membrane reactor is increased to 15% or more after the hydrothermal crystallization reaction.
Compared with the embodiment 2, the embodiment of the invention adopts nano Al2O3The sulfur capacity of the nano ZnO and nano CuO nano oxide system is up to more than 15%.
Meanwhile, the inventor research and development team finds that during the coprecipitation reaction, the gap between a rotor and a stator of the liquid membrane reactor is 10-20 microns, the shearing rate is 3000 rpm-5000 rpm, the reaction temperature is 40-50 ℃, the material flow rate is 100 kg/h-150 kg/h, the crystallization temperature is 140-150 ℃, the crystallization time is 20-35 min, and the sulfur capacity of the nano desulfurizer obtained by roasting the precursor at 400-500 ℃ for 4-5 h can be further increased to more than 20%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The nano desulfurizer is characterized by comprising nano Al2O3, nano ZnO and nano CuO, wherein the nano Al2O3The molar ratio of the nano ZnO to the nano CuO is as follows: (0.8-1.5): (0.8-1.5): (1.8-2.5).
2. The nano desulfurization agent according to claim 1, wherein the nano Al is2O3The molar ratio of the nano ZnO to the nano CuO is as follows: 1: 1: 2.
3. a method for preparing the nano desulfurizing agent according to any one of 1 to 2, which is characterized by comprising the following steps:
step S1: mixing the mixed ionic solution and a precipitator in a rotary liquid membrane reactor under high-speed shearing and carrying out coprecipitation reaction to obtain a coprecipitation reactant;
step S2: carrying out hydrothermal crystallization reaction on the coprecipitation reactant, and removing impurities to obtain a first precipitate;
step S3: forming the first precipitate, and drying to obtain a precursor;
step S4: roasting the precursor to obtain the nano desulfurizer;
wherein the mixed ion solution comprises Al3+,Zn2+And Cu2+Said Al3+,Zn2+And Cu2+The molar ratio of (1.6-3): (0.8-1.5): (1.8-2.5).
4. The method for preparing nano desulfurization agent according to claim 3, wherein in step S1, the precipitating agent is K2CO3Solution and/or Na2CO3A solution; wherein CO in the precipitant3 2-The metal ions in the mixed ion solution can be completely precipitated.
5. The method for preparing a nano desulfurizing agent according to claim 3, wherein the gap between the rotor and the stator of the rotary liquid membrane reactor is 10 μm to 30 μm, the shear rate is 2000rpm to 5000rpm, the reaction temperature is 30 ℃ to 60 ℃, and the material flow rate is 100kg/h to 150 kg/h.
6. The method for preparing a nano desulfurizing agent according to claim 3, wherein in the step S2, the crystallization temperature is 100 ℃ to 180 ℃ and the crystallization time is 10min to 60 min.
7. The method for preparing a nano desulfurizer according to claim 3, wherein in the step S4, the precursor is calcined at 350 to 550 ℃ for 2 to 5 hours to obtain the nano desulfurizer.
8. The method for preparing a nano desulfurizer as claimed in claim 3, wherein in the step S1, the gap between the rotor and the stator of the rotary liquid film reactor is 10 to 20 μm, the shear rate is 3000rpm to 5000rpm, the reaction temperature is 40 ℃ to 50 ℃, and the material flow rate is 100kg/h to 150 kg/h;
in the step S2, the crystallization temperature is 140-150 ℃, and the crystallization time is 20-35 min;
in the step S4, the precursor is roasted for 4 to 5 hours at the temperature of 400 to 500 ℃ to obtain the nano desulfurizer.
9. The reaction system for preparing the nano desulfurizer is characterized by comprising a rotary liquid film reactor and a tubular crystallization reactor which are sequentially connected, wherein the rotary liquid film reactor is used for mixing a mixed ionic solution and a precipitator under high-speed shearing and carrying out coprecipitation reaction, and the tubular crystallization reactor is used for carrying out hydrothermal crystallization reaction on a coprecipitation reactant.
10. The reaction system of a nano desulfurization agent according to claim 9, wherein the rotary liquid membrane reactor comprises:
the static disc is provided with a feeding hole;
the movable disc is arranged outside the static disc, an adjustable gap is formed between the movable disc and the static disc, and the movable disc can rotate relative to the static disc;
the closed disc is arranged on the opposite side of the movable disc, a gap opening between the movable disc and the static disc is closed, and a discharge hole is formed in the gap opening of the closed disc;
and
the feeding pipe is connected with the feeding hole and comprises a first feeding pipe and a second feeding pipe which are embedded inside and outside;
wherein the adjustable gap is in the range of 5-200 μm.
CN202011594178.5A 2020-12-29 2020-12-29 Nano desulfurizer, preparation method and reaction system Pending CN112604491A (en)

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