Calcination reduction process for catalyst

Abstract

The invention discloses a catalyst calcination reduction process which comprises the following steps: in an air environment, carrying out three-stage calcination on raw materials in a calcination reduction furnace at three-stage temperature, directly discharging no condensate water, and ending the calcination; replacing the calcining reduction furnace with nitrogen, and completing the replacement when the oxygen content monitor displays 0; cooling to 260-300 DEG C, opening the calcining reduction furnace, reducing the material in the furnace by hydrogen, gradually increasing the temperature of the calcining reduction furnace, controlling the temperature of the reduction furnace to be 390-420 DEG C, and ending the reduction of the catalyst when no water is discharged from the reduction furnace; (4) closing the hydrogen, calcining a reduction furnace heating system, and cooling; and (5) discharging and packaging when the temperature is reduced to 60-150 DEG C. Calcination and reduction are carried out in one device, the cost can be saved, the production efficiency can be improved, the damage to the mechanical stress of granular (honeycomb-shaped) products caused by temperature rise is avoided by adopting segmented calcination and segmented reduction, and the stability of the framework structure of the powder-state catalyst is ensured.

Description

Technical Field

[0001] The invention relates to a basic nickel carbonate processing technology, and in particular to a catalyst calcination reduction process. Background Art

[0002] In 2012, CNOOC Tianjin Chemical Research and Design Institute successfully developed a fat hydrogenation catalyst to fill the domestic gap. The construction of new hydrogenation catalyst production can provide necessary support conditions for the fat hydrogenation catalyst with independent intellectual property rights to quickly occupy the market. Based on this, the present invention is designed. Summary of the invention

[0003] In view of the problems existing in the prior art, the present invention proposes a catalyst calcination and reduction process. Calcination and reduction are carried out in one device, which can save costs and improve production efficiency. The use of staged calcination and staged reduction avoids the damage to the mechanical stress of the granular (honeycomb) product caused by the increase in temperature, and ensures the stability of the skeleton structure of the powdered catalyst.

[0004] The technical solution adopted by the present invention is: a catalyst calcination reduction process, comprising the following process steps: (1) In an air environment, the raw materials in the calcination reduction furnace are calcined in three stages at three temperatures. The electric heater of the calcination reduction furnace is turned on to heat the reduction furnace. The temperature is gradually increased to 420°C at room temperature and maintained between 400-420°C. During this period, three stages of calcination are performed at 100-130°C, 200-260°C, and 400-420°C. The first and second stages are respectively kept for 0.5-1 hour. The calcination is terminated directly without condensed water discharge; (2) Turn off the air, turn on the nitrogen to replace the calcination reduction furnace, and observe the oxygen content monitor. When the oxygen content monitor shows 0, the replacement is completed; (3) After the replacement is completed, the nitrogen flow rate is controlled at 10-25m³ / h, and the cooling system of the calcination reduction furnace is turned on to cool down. When the temperature drops to 260-300℃, the calcination reduction furnace is turned on to reduce the materials in the furnace with hydrogen. The temperature of the calcination reduction furnace is gradually increased and controlled between 390-420℃. During this period, the nitrogen-hydrogen ratio and temperature are continuously adjusted according to the drainage of the calcination reduction furnace. When no water is discharged from the reduction furnace, the catalyst reduction is completed; (5) Turn off the hydrogen and calcination reduction furnace heating systems, control the nitrogen flow rate to 10-15 m³ / h, and turn on the cooling system for cooling; (6) When the temperature drops to 6-150℃, unload and package.

[0005] Based on the above solution, as a preferred embodiment, before executing step (1), the following processing is performed: Start the calcination reduction furnace and stir; The raw materials are sucked into the calcination reduction furnace by negative pressure suction; Turn on the calcination reduction furnace air.

[0006] On the basis of the above scheme, as a preferred embodiment, the raw material intake amount is 150-200kg; the air flow rate is adjusted to 10-30m³ / h.

[0007] Based on the above scheme, as a preferred embodiment, in step (1), the heater output power is gradually adjusted according to the water output of the calcination reduction furnace to control the temperature (the water output changes from small to large and then to small, and the output power changes from small to large and then to small, and the temperature is maintained when it changes to small).

[0008] Based on the above scheme, preferably, in step (3), the temperature is maintained at 200-300°C for 0.5-1 hour, and the hydrogen flow rate is controlled between 5-20m³ / h.

[0009] On the basis of the above scheme, as a preferred embodiment, in step (3), the nitrogen-hydrogen ratio is continuously adjusted according to the drainage situation of the calcination reduction furnace, with a drainage volume of 1KG / H and a ratio of 1:4-1.

[0010] Based on the above scheme, preferably, in step (5), after the hydrogen is turned off, the nitrogen is maintained at 10-25m³ / h.

[0011] Compared with the prior art, the present invention has the following beneficial effects: The degree of automation is high, and there is no such technology at home or abroad.

[0012] Calcination and reduction are carried out in one device, which can save costs and improve production efficiency.

[0013] The use of staged calcination and staged reduction avoids the damage to the mechanical stress of the granular (honeycomb) product caused by the increase in temperature, and ensures the stability of the skeleton structure of the powdered catalyst.

[0014] Reduce catalyst agglomeration during calcination and reduction. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a structural schematic diagram of the present invention. DETAILED DESCRIPTION

[0016] The present invention will be further described below by way of examples, but the scope of the present invention is not limited thereto.

[0017] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit exemplary embodiments according to the present invention. As used herein, unless the context clearly indicates otherwise, the singular form is also intended to include the plural form. In addition, it should be understood that when the terms "comprising" and / or "including" are used in this specification, it indicates the presence of features, steps, operations, devices, components and / or combinations thereof.

[0018] The raw material catalyst targeted by the present invention comprises: main components of basic nickel carbonate, a carrier, hydrogen, air and nitrogen.

[0019] Process principle: Calcination decomposition: NiCO3→NiO+CO2 (endothermic reaction) Ni(HCO3)2→NiO+H2O+CO2 (endothermic reaction) Reduction stage: NiO+H2→Ni+H2O (endothermic reaction).

[0020] Applied equipment such as Figure 1 As shown, the catalyst calcination and reduction device includes a calcination and reduction furnace 1, the air inlet at the bottom of the calcination and reduction furnace is connected to an air source 2, a nitrogen source 3, and a hydrogen source 4 through a multi-way pipe, an oxygen content detector 6 is installed on the discharge pipeline 5 at the upper end of the calcination and reduction furnace, the end of the discharge pipeline is connected to a steam-water separator 7, one outlet of the steam-water separator is emptied, and the other outlet is connected to a drain pipe, a cylinder 8 loaded with catalyst is connected to the calcination and reduction furnace through a pipeline, and the bottom of the calcination and reduction furnace is connected to a discharge 9.

[0021] The specific process is as follows: A catalyst calcination reduction process: 1. Start the reduction furnace and stir; 2. The precursor basic nickel carbonate is sucked into the calcination reduction furnace by negative pressure suction, with the suction amount of 150-200kg; 3. Open the calcination reduction furnace air and adjust the air flow rate to 10-30m³ / h; 4. Turn on the electric heater of the calcination reduction furnace to heat the reduction furnace. The heating temperature is controlled to be between room temperature and gradually increased to 420℃, and maintained between 400-420℃. During this period, calcination is carried out in stages, with three stages of calcination at 100-130℃, 200-260℃, and 400-420℃. The first stage calcination treats dissolved water, the second stage calcination treats crystallized water, and the third stage calcination treats water produced by decomposition. The first and second stages stay for 0.5-1 hour respectively. According to the water output of the calcination reduction furnace, the output power of the heater is gradually adjusted to control the temperature. 5. After no condensed water is discharged from the calcination reduction furnace, the calcination is finished, the air is turned off, and the nitrogen is turned on to replace the calcination reduction furnace. Observe the oxygen content monitor. When the oxygen content monitor shows 0, the replacement is completed; 6. After the replacement is completed, control the nitrogen flow rate at 10-25m³ / h; turn on the cooling system of the calcination reduction furnace to cool down; 7. When the temperature drops to 260-300℃, open the calcination reduction furnace to reduce the materials in the furnace with hydrogen, and keep it for 0.5-1 hour; the hydrogen flow rate is controlled between 5-20m³ / h; 8. Gradually increase the temperature of the calcination reduction furnace and control the reduction temperature between 390-420℃ for 1.5-2 hours; 9. During the process, the nitrogen-hydrogen ratio and temperature are continuously adjusted according to the drainage of the calcination reduction furnace. When no water is discharged from the reduction furnace, the catalyst reduction is completed; the nitrogen-hydrogen ratio is adjusted between 1:4-1, and the amount of hydrogen is increased or decreased with the instantaneous flow rate of 1kg / h of drainage as a reference; 10. Turn off the hydrogen and calcination reduction furnace heating systems, control the nitrogen flow rate to 10-15 m³ / h, turn on the cooling system to cool down; maintain nitrogen at 10-25 m³ / h; 11. When the temperature drops to 60-150℃ (adjust the temperature according to the needs of different products), unload and package.

[0022] It should be noted that the embodiments described above are only used to explain the present invention and do not constitute any limitation to the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory words, rather than restrictive words. The present invention may be modified as specified within the scope of the claims of the present invention, and the present invention may be revised without departing from the scope and spirit of the present invention. Although the present invention described therein relates to specific methods, materials and embodiments, it does not mean that the present invention is limited to the specific examples disclosed therein, on the contrary, the present invention can be extended to all other methods and applications with the same functions.

Claims

1. A catalyst calcination reduction process, characterized in that: Including process steps: (1) In an air environment, the raw materials in the calcination reduction furnace are calcined in three stages at three temperatures. The electric heater of the calcination reduction furnace is turned on to heat the reduction furnace, gradually increasing from room temperature to 420°C, and controlling the temperature between 400-420°C. During this period, three stages of calcination are carried out at 100-130°C, 200-260°C, and 400-420°C. The first and second stages are respectively kept for 0.5-1 hour, and the calcination is terminated directly without condensed water discharge; (2) Turn off the air, turn on the nitrogen to replace the calcination reduction furnace, and observe the oxygen content monitor. When the oxygen content monitor shows 0, the replacement is completed; (3) After the replacement is completed, the nitrogen flow rate is controlled at 10-25m³ / h, and the cooling system of the calcination reduction furnace is turned on to cool down. When the temperature drops to 260-300°C, the calcination reduction furnace is turned on to reduce the materials in the furnace with hydrogen. The temperature of the calcination reduction furnace is gradually increased and controlled between 390-420°C. During this period, the nitrogen-hydrogen ratio and temperature are continuously adjusted according to the drainage of the calcination reduction furnace. When no water is discharged from the reduction furnace, the catalyst reduction is completed; (4) Turn off the hydrogen and calcination reduction furnace heating systems, control the nitrogen flow rate to 10-15 m³ / h, and turn on the cooling system for cooling; (5) Unload and package when the temperature drops to 60-150℃.

2. A catalyst calcination reduction process as claimed in claim 1, characterized in that: Before executing step (1), perform the following processing: Start the calcination reduction furnace and stir; The raw materials are sucked into the calcination reduction furnace by negative pressure suction; Turn on the calcination reduction furnace air.

3. A catalyst calcination reduction process as claimed in claim 2, characterized in that: The raw material intake is 150-200kg; the air flow is adjusted to 10-30m³ / h.

4. A catalyst calcination reduction process as claimed in claim 1, characterized in that: In step (1), the output power of the heater is gradually adjusted according to the water output of the calcination reduction furnace to control the temperature.

5. A catalyst calcination reduction process as claimed in claim 1, characterized in that: In step (3), the temperature is maintained at 260-300°C for 0.5-1 hour, and the hydrogen flow rate is controlled between 5-20 m³ / h.

6. A catalyst calcination reduction process as claimed in claim 1, characterized in that: In step (3), the nitrogen-hydrogen ratio is continuously adjusted according to the drainage situation of the calcination reduction furnace, with a drainage volume of 1 kg / h and a ratio of 1:4-1.

7. A catalyst calcination reduction process as claimed in claim 1, characterized in that: In step (5), after the hydrogen is turned off, the nitrogen is maintained at 10-25 m³ / h.

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