CN110756123A - Device and method for synthesizing catalyst by novel oxidation-reduction coprecipitation method - Google Patents

Device and method for synthesizing catalyst by novel oxidation-reduction coprecipitation method Download PDF

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CN110756123A
CN110756123A CN201910859787.XA CN201910859787A CN110756123A CN 110756123 A CN110756123 A CN 110756123A CN 201910859787 A CN201910859787 A CN 201910859787A CN 110756123 A CN110756123 A CN 110756123A
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solution
injection pump
reaction tank
catalyst
probe
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仲柳
方庆艳
李�权
张�成
陈刚
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Huazhong University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00054—Controlling or regulating the heat exchange system
    • B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058—Temperature measurement
    • B01J2219/00063—Temperature measurement of the reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00177—Controlling or regulating processes controlling the pH

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The invention discloses a device for synthesizing a catalyst by a novel oxidation-reduction coprecipitation method, which is characterized in that: comprises a reaction tank (1), an oxidant solution injection pump (2), a reducing agent solution injection pump (3), an alkali solution injection pump (4), a pH probe (5), a temperature probe (6), an upper computer (7) and a magnetic stirrer (8) with a heating function; the upper computer (7) controls the ion concentration and the oxidation-reduction reaction speed in the reaction tank (1) by controlling the advancing speeds of the oxidant solution injection pump (2) and the reducing agent solution injection pump (3), and accurately measures the pH value of the solution through a pH probe (5) in the reaction tank (1), and controls the advancing speed of the alkaline solution injection pump (4), so that the pH value of the prepared solution is stabilized in a preset range of the set pH value. The invention can control the pH value in the reaction tank with high precision, thereby controlling the synthesis reaction speed; the automation degree is high, and the manual error is reduced.

Description

Device and method for synthesizing catalyst by novel oxidation-reduction coprecipitation method
Technical Field
The invention belongs to the technical field of catalyst synthesis equipment, and particularly relates to a device and a method for synthesizing a catalyst by a novel oxidation-reduction coprecipitation method.
Background
With the rapid development of socioeconomic, the catalyst has gained a great deal of application in industrial production. The synthesis of catalysts with specific morphology and function is widely recognized. At present, a hydrothermal synthesis method, a coprecipitation method, a sol-gel method and an impregnation method are four synthesis methods which are used more, compared with other preparation methods, the coprecipitation method has wide application in industry because the process is simple and the requirement on the manufacturing environment is low, but the addition of a precipitator can cause the local pH value to be too high and destroy the precipitation kinetic balance, so that agglomeration is generated to cause uneven distribution of catalyst components, further the distribution of active sites of the catalyst on the surface of the catalyst is reduced, and the activity of the catalyst is reduced.
Disclosure of Invention
Aiming at least one of the defects or the improvement requirements of the prior art, the invention provides a device for synthesizing a catalyst by a novel oxidation-reduction coprecipitation method, which can control the local fluctuation of the concentration and the pH value of reactants in a reaction tank by controlling the speed of an oxidant solution, a reducing agent solution and an alkali solution, so as to achieve the purpose of controlling the generation speed of a precipitate, further achieve the purposes of reducing catalyst agglomeration and uniformly distributing different components.
To achieve the above objects, according to one aspect of the present invention, there is provided an apparatus for synthesizing a catalyst by a novel redox coprecipitation method, in which: comprises a reaction tank, an oxidant solution injection pump, a reducing agent solution injection pump, an alkali solution injection pump, a pH probe, a temperature probe, an upper computer and a magnetic stirrer with a heating function;
three injection pumps inject reactants into the reaction tank under the control of the upper computer;
the pH probe and the temperature probe are placed in the reaction tank and are respectively connected with the upper computer and the magnetic stirrer with the heating function;
the upper computer controls the ion concentration and the oxidation-reduction reaction speed in the reaction tank by controlling the propulsion speeds of the oxidant solution injection pump and the reducing agent solution injection pump, and controls the propulsion speed of the alkali solution injection pump by accurately measuring the pH value of the solution through a pH probe in the reaction tank, so that the pH value of the prepared solution is stabilized within a preset range of a set pH value;
and the magnetic stirrer with the heating function adjusts the temperature of the solution in the reaction tank through the real-time measurement result of the temperature probe, and stirs the solution in the reaction tank to uniformly mix the solution.
Preferably, the reaction tank is an open reaction tank.
Preferably, the oxidant solution injection pump, the reducing agent solution injection pump and the alkali solution injection pump all adopt a propulsion mode of a stepping motor with a neural network fuzzy PID controller.
Preferably, the oxidant solution injection pump, the reducing agent solution injection pump and the alkaline solution injection pump all have adaptive propulsion to balance resistance during travel.
Preferably, the neural network fuzzy PID controller respectively controls the propelling speeds of the three injection pumps according to different types and concentrations of the oxidant solution, the reducing agent solution and the alkali solution.
Preferably, the pH probe adopts a water-based pH probe or a resin pH probe.
Preferably, when the heating temperature of the solution in the reaction tank is higher than 80 ℃, the pH probe adopts a resin type pH probe;
when the heating temperature of the solution in the reaction tank is equal to or lower than 80 ℃, the pH probe adopts a water system pH probe.
Preferably, the material of the reaction tank is quartz glass or polytetrafluoroethylene.
Preferably, the oxidizer solution injection pump is made of polytetrafluoroethylene material.
In order to achieve the above objects, according to another aspect of the present invention, there is also provided a method for synthesizing a catalyst by a novel redox coprecipitation method, in which: the device for synthesizing the catalyst by the novel oxidation-reduction coprecipitation method is adopted, and comprises the following steps:
s1, preparing an acidic deionized water solution A, and weighing Mn (NO) with a predetermined mass3)250wt％H2Dissolving O in the solution A to obtain a solution B, and sucking the solution B into a reducing solution injection pump;
s2, preparing an acidic deionized water solution C, and weighing KMnO with a predetermined mass4Solid and predetermined mass of (NH)4)2Ce(NO3)6Adding the solution D into the solution C, stirring to dissolve the solution C to obtain a solution D, and sucking the solution D into an oxidizing solution injection pump;
s3, preparing a predetermined amount of KOH solution E, and sucking the solution E into an alkali solution injection pump;
s4, starting a magnetic stirrer with a heating function, heating the deionized water in the reaction tank to a preset heating temperature, and starting magnetic stirring;
s5, setting a pH value required by the catalyst synthesis on an upper computer, starting the three injection pumps to work, and injecting a reaction chemical solution into a reaction tank;
s6, continuing to stir for a preset time, and standing and aging for a preset time; the required catalyst is obtained by filtering, washing, drying and roasting.
The above-described preferred features may be combined with each other as long as they do not conflict with each other.
Generally, compared with the prior art, the above technical solution conceived by the present invention has the following beneficial effects:
1. the device and the method for synthesizing the catalyst by the novel oxidation-reduction co-precipitation method can control the local fluctuation of the concentration and the pH value of reactants in a reaction tank by controlling the speed of an oxidant solution, a reducing agent solution and an alkali solution, achieve the aim of controlling the generation speed of the precipitate, and further achieve the aims of reducing catalyst agglomeration and uniformly distributing different components.
2. The device and the method for synthesizing the catalyst by the novel oxidation-reduction coprecipitation method have the advantages of advanced logic structure design; the degree of automation is high, reduces artifical error, has reaction solution pH stability, catalyst synthesis homogeneous advantage.
Drawings
FIG. 1 is a schematic diagram of the structure of an apparatus for synthesizing a catalyst by a novel redox coprecipitation process according to the invention;
FIG. 2 is a graph showing pH fluctuations in a reaction tank of three examples of the novel method for synthesizing a catalyst by a co-redox precipitation method according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other. The present invention will be described in further detail with reference to specific embodiments.
As a preferred embodiment of the present invention, as shown in fig. 1, the present invention provides an apparatus for synthesizing a catalyst by a novel redox coprecipitation method, wherein: comprises a reaction tank 1, an oxidant solution injection pump 2, a reducing agent solution injection pump 3, an alkali solution injection pump 4, a pH probe 5, a temperature probe 6, an upper computer 7 and a magnetic stirrer 8 with a heating function.
Three injection pumps inject reactants into the reaction tank 1 under the control of the upper computer 7;
the pH probe 5 and the temperature probe 6 are arranged in the reaction tank 1 and are respectively connected with the upper computer 7 and the magnetic stirrer 8 with the heating function;
the upper computer 7 controls the ion concentration and the oxidation-reduction reaction speed in the reaction tank 1 by controlling the advancing speeds of the oxidant solution injection pump 2 and the reducing agent solution injection pump 3, accurately measures the pH value of the solution through a pH probe 5 in the reaction tank 1, and controls the advancing speed of the alkali solution injection pump 4 through a neural network algorithm, so that the pH value of the prepared solution is stabilized within a preset range of a set pH value;
the magnetic stirrer 8 with the heating function adjusts the temperature of the solution in the reaction tank through the real-time measurement result of the temperature probe 6, and stirs the solution in the reaction tank at a certain speed so as to uniformly mix the solution.
The reaction tank 1 is one of open reaction tanks such as an open beaker and a flask. The material of the reaction tank 1 is acid-resistant and oxidation-resistant material, including quartz glass and polytetrafluoroethylene, and quartz glass is preferred in view of cost.
The oxidizer solution injection pump 2 is made of a material having high mechanical strength and oxidation resistance, and preferably made of polytetrafluoroethylene in view of sealing property; the injection pumps of the reducing agent solution injection pump 3 and the alkali solution injection pump 4 are common injection pumps with high mechanical strength. The syringe pump has sufficient tightness to ensure that all the solution enters the reaction tank.
The oxidant solution injection pump 2, the reducing agent solution injection pump 3 and the alkali solution injection pump 4 are all in a propulsion mode of a stepping motor with a neural network fuzzy PID controller. The oxidant solution injection pump 2, the reducing agent solution injection pump 3 and the alkali solution injection pump 4 are provided with self-adaptive driving forces for balancing resistance in the advancing process. The control logic of the stepping motor is calculated by a large amount of data to ensure that the injection pump can be self-adapted to various different oxidants, different reducing agents, different alkali solutions and respective different concentrations; the neural network fuzzy PID controller respectively controls the propelling speeds of the three injection pumps according to different types and concentrations of an oxidant solution, a reducing agent solution and an alkali solution.
The upper computer 7 accurately measures the pH value of the solution through a high-precision pH probe 5 arranged in the reaction tank 1, and stabilizes the pH value of the prepared solution near a set value by controlling the propelling speeds of the oxidant injection pump 2, the reducing agent injection pump 3 and the alkali solution injection pump 4.
The high-precision pH probe 5 can adopt a water system pH probe and a resin pH probe: when the heating temperature of the solution in the reaction tank is higher than 80 ℃, the pH probe 5 adopts a resin type pH probe; when the heating temperature of the solution in the reaction tank is equal to or lower than 80 ℃, the pH probe 5 adopts a water system pH probe.
Stirring and heating the reaction solution in the reaction tank by a magnetic stirrer 8 with a heating function, and further realizing the constant-temperature uniform reaction of the solution; the heating function of the magnetic stirrer is realized by the measurement feedback of the temperature probe 6 and the regulation of the temperature controller of the stirrer.
The invention relates to a method for synthesizing a catalyst by a novel oxidation-reduction coprecipitation method, wherein the method comprises the following steps: the device for synthesizing the catalyst by the novel oxidation-reduction coprecipitation method is adopted, and comprises the following steps:
s1, preparing an acidic deionized water solution A, and weighing Mn (NO) with a predetermined mass3)250wt％H2Dissolving O in the solution A to obtain a solution B, and sucking the solution B into a reducing solution injection pump 3;
s2, preparing an acidic deionized water solution C, and weighing KMnO with a predetermined mass4Solid and predetermined mass of (NH)4)2Ce(NO3)6Adding the solution D into the solution C, stirring to dissolve the solution C to obtain a solution D, and sucking the solution D into an oxidizing solution injection pump 2;
s3, preparing a predetermined amount of KOH solution E, and sucking the solution E into the alkaline solution injection pump 4;
s4, starting a magnetic stirrer 8 with a heating function, heating deionized water in the reaction tank to a preset heating temperature, and starting magnetic stirring;
s5, setting a pH value required by the catalyst synthesis on the upper computer 7, starting the three injection pumps to work, and injecting a reaction chemical solution into the reaction tank;
s6, continuing to stir for a preset time, and standing and aging for a preset time; the required catalyst is obtained by filtering, washing, drying and roasting.
The method for synthesizing the catalyst by the novel oxidation-reduction coprecipitation method of the invention provides a plurality of examples, and the fluctuation situation of pH in a reaction tank is shown in figure 2.
Example 1
Acid (nitric acid) deionized water solution a (pH 1.0) was prepared, and 9.31g of Mn (NO) was weighed out3)250wt％H2Dissolving O in the solution A to obtain a solutionB, sucking the solution B into a reducing solution injection pump 3;
acid (nitric acid) deionized water solution C (pH 1.0) was prepared, and 2.78g KMnO was weighed in4Solids and 2.69g (NH)4)2Ce(NO3)6Adding the solution D into the solution C, stirring to dissolve the solution C to obtain a solution D, and sucking the solution D into an oxidizing solution injection pump 2;
preparing 0.4M KOH solution E (pH is 13.6), and sucking the solution E into an alkali solution injection pump 4;
starting a magnetic stirrer 8 with a heating function, heating deionized water in the reaction tank to 70 ℃, and starting magnetic stirring;
setting the pH value (1.0) required by the catalyst synthesis on an upper computer 7, starting the operation of an injection pump, and injecting a reaction chemical solution into a reaction tank;
after the end, stirring is continued for 30min, and the mixture is kept still and aged for 30 min. Filtering with a vacuum suction filter pump to obtain a filter cake, and alternately washing with deionized water and absolute ethyl alcohol for more than 3 times; the filter cake was dried in a drying oven at 105 ℃ for 12 hours and then calcined in a muffle furnace (air atmosphere) at 500 ℃ to give the desired catalyst.
Example 2
Acid (nitric acid) deionized water solution a (pH 1.0) was prepared, and 9.31g of Mn (NO) was weighed out3)250wt％H2Dissolving O in the solution A to obtain a solution B, and sucking the solution B into a reducing solution injection pump 3;
acid (nitric acid) deionized water solution C (pH 1.0) was prepared, and 2.78g KMnO was weighed in4Solids and 2.69g (NH)4)2Ce(NO3)6Adding the solution D into the solution C, stirring to dissolve the solution C to obtain a solution D, and sucking the solution D into an oxidizing solution injection pump 2;
preparing 0.4M KOH solution E (pH is 13.6), and sucking the solution E into an alkali solution injection pump 4;
starting a magnetic stirrer 8 with a heating function, heating deionized water in the reaction tank to 70 ℃, and starting magnetic stirring;
setting the pH value (3.0) required by the catalyst synthesis on an upper computer 7, starting the operation of an injection pump, and injecting a reaction chemical solution into a reaction tank;
after the end, stirring is continued for 30min, and the mixture is kept still and aged for 30 min. Filtering with a vacuum suction filter pump to obtain a filter cake, and alternately washing with deionized water and absolute ethyl alcohol for more than 3 times; the filter cake was dried in a drying oven at 105 ℃ for 12 hours and then calcined in a muffle furnace (air atmosphere) at 500 ℃ to give the desired catalyst.
Example 3
Acid (nitric acid) deionized water solution a (pH 1.0) was prepared, and 9.31g of Mn (NO) was weighed out3)250wt％H2Dissolving O in the solution A to obtain a solution B, and sucking the solution B into a reducing solution injection pump 3;
acid (nitric acid) deionized water solution C (pH 1.0) was prepared, and 2.78g KMnO was weighed in4Solids and 2.69g (NH)4)2Ce(NO3)6Adding the solution D into the solution C, stirring to dissolve the solution C to obtain a solution D, and sucking the solution D into an oxidizing solution injection pump 2;
preparing 0.4M KOH solution E (pH is 13.6), and sucking the solution E into an alkali solution injection pump 4;
starting a magnetic stirrer 8 with a heating function, heating deionized water in the reaction tank to 70 ℃, and starting magnetic stirring;
setting the pH value (5.0) required by the catalyst synthesis on an upper computer 7, starting the operation of an injection pump, and injecting a reaction chemical solution into a reaction tank;
after the end, stirring is continued for 30min, and the mixture is kept still and aged for 30 min. Filtering with a vacuum suction filter pump to obtain a filter cake, and alternately washing with deionized water and absolute ethyl alcohol for more than 3 times; the filter cake was dried in a drying oven at 105 ℃ for 12 hours and then calcined in a muffle furnace (air atmosphere) at 500 ℃ to give the desired catalyst.
In summary, the invention has the following advantages:
the device and the method for synthesizing the catalyst by the novel oxidation-reduction co-precipitation method can control the local fluctuation of the concentration and the pH value of reactants in a reaction tank by controlling the speed of an oxidant solution, a reducing agent solution and an alkali solution, achieve the aim of controlling the generation speed of the precipitate, and further achieve the aims of reducing catalyst agglomeration and uniformly distributing different components.
The device and the method for synthesizing the catalyst by the novel oxidation-reduction coprecipitation method have the advantages of advanced logic structure design; the degree of automation is high, reduces artifical error, has reaction solution pH stability, catalyst synthesis homogeneous advantage.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A device for synthesizing a catalyst by a novel oxidation-reduction coprecipitation method is characterized in that:
comprises a reaction tank (1), an oxidant solution injection pump (2), a reducing agent solution injection pump (3), an alkali solution injection pump (4), a pH probe (5), a temperature probe (6), an upper computer (7) and a magnetic stirrer (8) with a heating function;
three injection pumps are controlled by the upper computer (7) to inject reactants into the reaction tank (1);
the pH probe (5) and the temperature probe (6) are placed in the reaction tank (1) and are respectively connected with the upper computer (7) and the magnetic stirrer (8) with the heating function;
the upper computer (7) controls the ion concentration and the oxidation-reduction reaction speed in the reaction tank (1) by controlling the advancing speeds of the oxidant solution injection pump (2) and the reducing agent solution injection pump (3), and controls the advancing speed of the alkali solution injection pump (4) by accurately measuring the pH value of the solution through a pH probe (5) in the reaction tank (1), so that the pH value of the prepared solution is stabilized within a preset range of a set pH value;
and the magnetic stirrer (8) with the heating function adjusts the temperature of the solution in the reaction tank through the real-time measurement result of the temperature probe (6), and stirs the solution in the reaction tank to uniformly mix the solution.
2. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 1, wherein:
the reaction tank (1) is an open reaction tank.
3. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 1, wherein:
the oxidant solution injection pump (2), the reducing agent solution injection pump (3) and the alkali solution injection pump (4) are all in a propulsion mode of a stepping motor with a neural network fuzzy PID controller.
4. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 3, wherein:
the oxidant solution injection pump (2), the reducing agent solution injection pump (3) and the alkali solution injection pump (4) are provided with self-adaptive driving forces to balance resistance in the advancing process.
5. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 3, wherein:
the neural network fuzzy PID controller respectively controls the propelling speeds of the three injection pumps according to different types and concentrations of an oxidant solution, a reducing agent solution and an alkali solution.
6. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 1, wherein:
the pH probe (5) adopts a water system pH probe or a resin pH probe.
7. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 6, wherein:
when the heating temperature of the solution in the reaction tank is higher than 80 ℃, the pH probe (5) adopts a resin type pH probe;
when the heating temperature of the solution in the reaction tank is equal to or lower than 80 ℃, the pH probe (5) adopts a water-based pH probe.
8. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 1, wherein:
the reaction tank (1) is made of quartz glass or polytetrafluoroethylene.
9. The apparatus for synthesizing a catalyst by a novel redox coprecipitation method according to claim 1, wherein:
the oxidant solution injection pump (2) is made of polytetrafluoroethylene materials.
10. A novel method for synthesizing a catalyst by a redox coprecipitation method is characterized by comprising the following steps: an apparatus for the synthesis of a catalyst by a novel redox coprecipitation process according to any of claims 1 to 9, comprising the following steps:
s1, preparing an acidic deionized water solution A, and weighing Mn (NO) with a predetermined mass3)250wt％H2Dissolving O in the solution A to obtain a solution B, and sucking the solution B into a reducing solution injection pump (3);
s2, preparing an acidic deionized water solution C, and weighing KMnO with a predetermined mass4Solid and predetermined mass of (NH)4)2Ce(NO3)6Adding the solution D into the solution C, stirring to dissolve the solution C to obtain a solution D, and sucking the solution D into an oxidizing solution injection pump (2);
s3, preparing a predetermined amount of KOH solution E, and sucking the solution E into an alkali solution injection pump (4);
s4, starting a magnetic stirrer (8) with a heating function, heating the deionized water in the reaction tank to a preset heating temperature, and starting magnetic stirring;
s5, setting a pH value required by the catalyst synthesis on an upper computer (7), starting to work by three injection pumps, and injecting a reaction chemical solution into a reaction tank;
s6, continuing to stir for a preset time, and standing and aging for a preset time; the required catalyst is obtained by filtering, washing, drying and roasting.
CN201910859787.XA 2019-09-11 2019-09-11 Device and method for synthesizing catalyst by novel oxidation-reduction coprecipitation method Pending CN110756123A (en)

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Cited By (2)

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CN112782337A (en) * 2020-12-23 2021-05-11 聊城大学 Method for controlling variable in coprecipitation method and application
CN113230995A (en) * 2021-06-08 2021-08-10 安徽理工大学环境友好材料与职业健康研究院(芜湖) Parallel flow type coprecipitation reaction device

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Application publication date: 20200207