CN111233056A - Preparation method of poly-platinum oxide - Google Patents
Preparation method of poly-platinum oxide Download PDFInfo
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- CN111233056A CN111233056A CN202010054380.2A CN202010054380A CN111233056A CN 111233056 A CN111233056 A CN 111233056A CN 202010054380 A CN202010054380 A CN 202010054380A CN 111233056 A CN111233056 A CN 111233056A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/004—Oxides; Hydroxides
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
Abstract
The invention discloses a preparation method of a poly-platinum oxide, which comprises the following steps: step 1, adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension; adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution; step 2, adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then taking nitrogen as aeration gas, and flushing a reducing agent solution into the suspension for aeration reaction to obtain a poly-platinum oxide suspension; and 3, carrying out constant-temperature spray reaction on the poly-platinum oxide suspension, and collecting the poly-platinum oxide after the reaction is finished. According to the preparation method, hydrazine hydrate is formed through aeration to react with platinum oxide in a small amount and uniformly, a multi-platinum structure is maintained, and a multi-platinum oxide suspension is prepared; the particles are recycled through constant-temperature spraying of the turbid liquid, more multi-platinum oxides can be collected, the reaction process steps are simple, the raw material investment is low, and the method has good practical value.
Description
Technical Field
The invention belongs to the technical field of platinum oxides, and particularly relates to a preparation method of a poly-platinum oxide.
Background
The noble metal catalyst includes a supported noble metal catalyst and a noble metal compound, and generally, the catalytic activity of the noble metal catalyst is represented by the content of a noble metal element, and the noble metal content of platinum oxide is high, and a platinum oxygen compound having a higher platinum content is not present.
Platinum oxide is used for hydrogenation, hydrogenolysis, dehydrogenation and oxidation reactions; the platinum metal (platinum black) formed by the reduction in the reaction is an active catalyst. In the above applications, there still exist individual reactions which are difficult to catalyze or have low catalytic efficiency, and it is necessary to further increase the content of platinum in the catalyst to increase the catalytic activity, thereby achieving the purpose of smooth catalytic reaction.
Disclosure of Invention
The invention aims to provide a preparation method of a poly-platinum oxide, which is used for catalyzing the reaction that the existing platinum oxide is difficult to catalyze or has low catalysis efficiency.
The technical scheme adopted by the invention is that the preparation method of the poly-platinum oxide comprises the following steps:
step 1, raw material pretreatment
Adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension for later use;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution for later use;
step 2, preparing poly platinum oxide suspension
Adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then taking nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension;
and 3, carrying out constant-temperature spray reaction on the poly-platinum oxide suspension liquid obtained in the step 2, and collecting the poly-platinum oxide after the reaction is finished.
The present invention is also characterized in that,
in the step 1, the concentration of the platinum oxide in the suspension is 10-30g/L, and the molar ratio of hydrazine hydrate to the platinum oxide is 1: 3-5.
The ultrasonic reaction parameters in the step 1 are as follows: the ultrasonic frequency is 40-80kHz, and the ultrasonic temperature is 20-40 ℃.
In the step 1, the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.2-0.6;
the parameters of stirring were: the stirring temperature is 1-4 ℃, and the stirring speed is 2000-4000 r/min.
The aeration reaction parameters in the step 2 are as follows: the speed of aeration gas is 5-10ml/min, the temperature of suspension in the reaction is 80-100 ℃, and the pressure of the sealed reaction kettle is not more than 4 Mpa.
And 2, the volume ratio of the nitrogen to the reducing agent solution is 10-15: 2.
Step 2, constant-temperature spraying reaction parameters: the constant temperature is 120-;
the collection is specifically as follows: at the temperature of not lower than 100 ℃, naturally settling at constant temperature, filling nitrogen, relieving pressure and collecting.
The invention has the beneficial effects that: according to the preparation method of the poly-platinum oxide, hydrazine hydrate is formed through aeration to react with platinum oxide in a small amount and uniformly, a poly-platinum structure is maintained, and a poly-platinum oxide suspension is prepared; the particles are recycled through constant-temperature spraying of the turbid liquid, more multi-platinum oxides can be collected, the reaction process steps are simple, the raw material investment is low, and the method has good practical value.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments.
The invention relates to a preparation method of a poly-platinum oxide, which comprises the following steps:
step 1, raw material pretreatment
Adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension for later use; the concentration of platinum oxide in the suspension is 10-30 g/L;
the ultrasonic reaction parameters are as follows: the ultrasonic frequency is 40-80kHz, and the ultrasonic temperature is 20-40 ℃.
Adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution for later use; the molar ratio of hydrazine hydrate to platinum oxide is 1: 3-5; the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.2-0.6; the parameters of stirring were: the stirring temperature is 1-4 ℃, and the stirring speed is 2000-4000 r/min.
The temperature is set during the stirring process so as to control the reaction speed of the hydrazine hydrate solution rushing into the reaction kettle and the platinum oxide later, which is beneficial to maintaining a multi-platinum structure.
Step 2, preparing poly platinum oxide suspension
Adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then taking nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension;
the aeration reaction parameters are as follows: the speed of aeration gas is 5-10ml/min, the temperature of suspension in the reaction is 80-100 ℃, and the pressure of the sealed reaction kettle is not more than 4 Mpa.
The volume ratio of the nitrogen to the reducing agent solution is 10-15: 2.
In the hydrazine hydrate reduction reaction, the aeration reaction has the following functions: hydrazine hydrate can enter the reaction kettle in a dispersed manner, the property of the hydrazine hydrate is similar to that of stirring, and if the reducing agent and the aeration gas are flushed together, the hydrazine hydrate and the platinum oxide can be formed to have a small amount of uniform reaction, and a multi-platinum structure is maintained.
And 3, carrying out constant-temperature spray reaction on the poly-platinum oxide suspension liquid obtained in the step 2, wherein the aim is to recover particles through suspension liquid spray, and collecting the poly-platinum oxide after the reaction is finished.
Constant temperature spray reaction parameters: the constant temperature is 120-;
the specific collection method comprises the following steps: at the temperature of not lower than 100 ℃, naturally settling at constant temperature, filling nitrogen, relieving pressure and collecting.
Example 1
Step 1, adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension with the platinum oxide concentration of 10g/L, wherein the ultrasonic frequency is 40kHz, and the ultrasonic temperature is 20 ℃;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution; the molar ratio of hydrazine hydrate to platinum oxide is 1: 3; the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.2; wherein the stirring temperature is 1 ℃, and the stirring speed is 2000 r/min.
Step 2, adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then using nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension, wherein the volume ratio of nitrogen to the reducing agent solution is 10: 2;
the aeration reaction parameters are as follows: the speed of aeration gas is 5ml/min, the temperature of suspension in the reaction is 80 ℃, and the pressure of the sealed reaction kettle is 4 Mpa.
And 3, carrying out constant-temperature spraying reaction on the multi-platinum oxide suspension obtained in the step 2, wherein the constant-temperature spraying reaction parameters are as follows: the constant temperature is 120 ℃, and the spraying speed is 3 mL/min; after the reaction is finished, naturally settling at constant temperature at 100 ℃, filling nitrogen, releasing pressure, and collecting to obtain the poly-platinum oxide.
Example 2
Step 1, adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension liquid with the platinum oxide concentration of 30g/L, wherein the ultrasonic frequency is 80kHz, and the ultrasonic temperature is 40 ℃;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution; the molar ratio of hydrazine hydrate to platinum oxide is 1: 5; the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.6; wherein the stirring temperature is 4 ℃, and the stirring speed is 4000 r/min.
Step 2, adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then using nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension, wherein the volume ratio of the nitrogen to the reducing agent solution is 15: 2;
the aeration reaction parameters are as follows: the speed of aeration gas is 10ml/min, the temperature of suspension in the reaction is 100 ℃, and the pressure of the sealed reaction kettle is 3 Mpa.
And 3, carrying out constant-temperature spraying reaction on the multi-platinum oxide suspension obtained in the step 2, wherein the constant-temperature spraying reaction parameters are as follows: the constant temperature is 150 ℃, and the spraying speed is 7 mL/min; after the reaction is finished, naturally settling at constant temperature at 120 ℃, filling nitrogen, relieving pressure and collecting to obtain the poly-platinum oxide.
Example 3
Step 1, adding platinum oxide into distilled water, and uniformly dispersing by ultrasonic to obtain suspension with platinum oxide concentration of 15g/L, wherein the ultrasonic frequency is 50kHz and the ultrasonic temperature is 25 ℃;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution; the molar ratio of hydrazine hydrate to platinum oxide is 1: 3.5; the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.3; wherein the stirring temperature is 2 ℃, and the stirring speed is 2500 r/min.
Step 2, adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then using nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension, wherein the volume ratio of nitrogen to the reducing agent solution is 12: 2;
the aeration reaction parameters are as follows: the speed of aeration gas is 6ml/min, the temperature of suspension in the reaction is 90 ℃, and the pressure of the sealed reaction kettle is 3.2 Mpa.
And 3, carrying out constant-temperature spraying reaction on the multi-platinum oxide suspension obtained in the step 2, wherein the constant-temperature spraying reaction parameters are as follows: the constant temperature is 125 ℃, and the spraying speed is 4 mL/min; after the reaction is finished, naturally settling at a constant temperature at 105 ℃, filling nitrogen, relieving pressure and collecting to obtain the poly-platinum oxide.
Example 4
Step 1, adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension with platinum oxide concentration of 20g/L, wherein the ultrasonic frequency is 60kHz and the ultrasonic temperature is 30 ℃;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution; the molar ratio of hydrazine hydrate to platinum oxide is 1: 4; the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.4; wherein the stirring temperature is 3 ℃, and the stirring speed is 3000 r/min.
Step 2, adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then using nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension, wherein the volume ratio of the nitrogen to the reducing agent solution is 13: 2;
the aeration reaction parameters are as follows: the speed of aeration gas is 8ml/min, the temperature of suspension in the reaction is 90 ℃, and the pressure of the sealed reaction kettle is 2.5 Mpa.
And 3, carrying out constant-temperature spraying reaction on the multi-platinum oxide suspension obtained in the step 2, wherein the constant-temperature spraying reaction parameters are as follows: the constant temperature is 130 ℃, and the spraying speed is 5 mL/min; after the reaction is finished, naturally settling at constant temperature at 130 ℃, filling nitrogen, relieving pressure and collecting to obtain the poly-platinum oxide.
Example 5
Step 1, adding platinum oxide into distilled water, and uniformly dispersing by ultrasonic to obtain suspension with the platinum oxide concentration of 25g/L, wherein the ultrasonic frequency is 70kHz and the ultrasonic temperature is 35 ℃;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution; the molar ratio of hydrazine hydrate to platinum oxide is 1: 4.5; the volume ratio of hydrazine hydrate to absolute ethyl alcohol is 1: 0.5; wherein the stirring temperature is 3.5 ℃, and the stirring speed is 3500 r/min.
Step 2, adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air of the reaction kettle and filling nitrogen, then using nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension, wherein the volume ratio of the nitrogen to the reducing agent solution is 14: 2;
the aeration reaction parameters are as follows: the speed of aeration gas is 8ml/min, the temperature of suspension in the reaction is 90 ℃, and the pressure of the sealed reaction kettle is 3.5 Mpa.
And 3, carrying out constant-temperature spraying reaction on the multi-platinum oxide suspension obtained in the step 2, wherein the constant-temperature spraying reaction parameters are as follows: the constant temperature is 140 ℃, and the spraying speed is 6 mL/min; after the reaction is finished, naturally settling at constant temperature at 140 ℃, filling nitrogen, relieving pressure and collecting to obtain the poly-platinum oxide.
According to the poly-platinum oxide prepared in the embodiments 1-5, in the preparation process, the reaction process steps are simple, the raw material investment is low, hydrazine hydrate formed by aeration reacts with platinum oxide in a small amount and uniformly, a poly-platinum structure is maintained, and a poly-platinum oxide suspension is prepared; particles are recovered by constant-temperature spraying of the suspension, so that more polyplatinum oxide can be collected.
Claims (7)
1. A preparation method of a polyplatinum oxide is characterized by comprising the following steps:
step 1, raw material pretreatment
Adding platinum oxide into distilled water, and performing ultrasonic dispersion uniformly to obtain a suspension for later use;
adding hydrazine hydrate into absolute ethyl alcohol, and uniformly stirring to obtain a reducing agent solution for later use;
step 2, preparing poly platinum oxide suspension
Adding the suspension obtained in the step 1 into a sealed reaction kettle, evacuating the air in the reaction kettle and filling nitrogen, then taking nitrogen as aeration gas, and flushing the reducing agent solution obtained in the step 1 into the suspension for aeration reaction to obtain a poly-platinum oxide suspension;
and 3, carrying out constant-temperature spray reaction on the poly-platinum oxide suspension liquid obtained in the step 2, and collecting the poly-platinum oxide after the reaction is finished.
2. The method for preparing polyplatinum oxide according to claim 1, wherein the concentration of platinum oxide in the suspension in step 1 is 10-30g/L, and the molar ratio of hydrazine hydrate to platinum oxide is 1: 3-5.
3. The method for preparing polyplatinum oxide according to claim 1, wherein the ultrasonic reaction parameters in step 1 are as follows: the ultrasonic frequency is 40-80kHz, and the ultrasonic temperature is 20-40 ℃.
4. The method for preparing polyplatinum oxide according to claim 1, wherein the volume ratio of hydrazine hydrate to absolute ethyl alcohol in step 1 is 1: 0.2-0.6;
the stirring parameters are as follows: the stirring temperature is 1-4 ℃, and the stirring speed is 2000-4000 r/min.
5. The method for preparing polyplatinum oxide according to claim 1, wherein the aeration reaction parameters in step 2 are as follows: the speed of aeration gas is 5-10ml/min, the temperature of suspension in the reaction is 80-100 ℃, and the pressure of the sealed reaction kettle is not more than 4 Mpa.
6. The method for preparing polyplatinum oxide according to claim 1, wherein the volume ratio of the nitrogen gas to the reducing agent solution in step 2 is 10-15: 2.
7. The method for preparing polyplatinum oxide according to claim 1, wherein the constant temperature spraying reaction parameters in step 2 are as follows: the constant temperature is 120-;
the specific collection mode is as follows: at the temperature of not lower than 100 ℃, naturally settling at constant temperature, filling nitrogen, relieving pressure and collecting.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
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Application publication date: 20200605 |