Industrial grade grease catalyst vulcanization process

Abstract

Belonging to the technical field of industrial grease processing, the invention discloses an industrial grade grease catalyst vulcanization process, which comprises the following steps: selecting a mixture of molybdenum trioxide and nickel oxide as a catalyst, and adding the catalyst into a solid bed catalyst reactor to form a catalyst bed layer; introducing inert gas into the solid bed catalyst reactor, and removing air; a catalyst bed layer in the solid bed catalyst reactor is preheated through heating equipment of the solid bed catalyst reactor; selecting one or more of dimethyl disulfide (DMDS), carbon disulfide (CS2), dimethyl sulfide (DMS) and a composite DMDS vulcanizing agent as a vulcanizing agent, and introducing the vulcanizing agent into the fixed bed catalyst reactor; introducing cold hydrogen into the solid bed catalyst reactor; after vulcanization is completed, injection of the vulcanizing agent is stopped, a catalyst bed layer in the solid bed catalyst reactor is cooled to the room temperature, the catalytic efficiency can be achieved and guaranteed, and the activity of the catalyst is maintained.

Description

Technical Field

[0001] The present invention relates to the technical field of industrial oil processing, and more particularly to an industrial-grade oil catalyst vulcanization process. Background Art

[0002] As a green, low-carbon alternative energy source, biodiesel plays a key role in addressing the global energy crisis and environmental pollution. This R&D project, based on the hydrodeoxygenation of industrial-grade oils to produce second-generation biodiesel, focuses on high-efficiency catalyst design and process optimization, aiming to overcome the bottlenecks of traditional biodiesel production technology and achieve higher-quality, more economical product output.

[0003] In the industrial-grade hydrodeoxygenation process for oils and fats, the active components of the catalyst primarily exist in the oxidized form of metal elements. Currently used hydrodeoxygenation catalysts consist of molybdenum oxide (MoO3) and nickel oxide (NiO). Research indicates that catalyst activity is optimal when the metal elements are present in a sulfided form. Therefore, prior to commissioning, the catalyst must undergo a sulfidation treatment to activate its activity. However, during the sulfidation process, existing catalysts generate high temperatures, leading to sintering and a decrease in catalyst activity. This also reduces sulfidation efficiency. The following proposes a solution to these problems. Summary of the Invention

[0004] In view of the problems existing in the prior art, the purpose of the present invention is to provide an industrial-grade grease catalyst vulcanization process, which can ensure the catalytic efficiency and maintain the activity of the catalyst.

[0005] To solve the above problems, the present invention adopts the following technical solutions.

[0006] An industrial-grade grease catalyst vulcanization process comprises the following steps:

[0007] A. Select an industrial grease catalyst, select a mixture of molybdenum trioxide and nickel oxide as a catalyst, and add the catalyst into a solid bed catalyst reactor to form a catalyst bed;

[0008] B. Exhaust air: use inert gas to pass into the solid bed catalyst reactor to purge the catalyst bed and remove air;

[0009] C. Catalyst preheating: The catalyst bed inside the solid bed catalyst reactor is preheated by the heating equipment of the solid bed catalyst reactor itself. The temperature range is controlled between 100 degrees Celsius and 400 degrees Celsius, and the heating rate is between 10 degrees Celsius per hour and 30 degrees Celsius per hour;

[0010] D. Select a vulcanizing agent, select one or more of dimethyl disulfide (DMDS), carbon disulfide (CS2), dimethyl sulfide (DMS) and a composite DMDS vulcanizing agent as the vulcanizing agent, introduce the vulcanizing agent into the interior of the fixed bed catalyst reactor, control the injection pressure of the vulcanizing agent to be between 1 MPa and 2 MPa, and control the pressure inside the solid bed catalyst reactor to be between 1 MPa and 10 MPa;

[0011] E. At the beginning of step D, cold hydrogen is introduced into the solid bed catalyst reactor, and the temperature of the catalyst bed is monitored by a temperature sensor inside the solid bed catalyst reactor to maintain the temperature between 100 degrees Celsius and 400 degrees Celsius.

[0012] F. After the sulfurization is completed, the injection of the sulfurizing agent is stopped and the catalyst bed inside the solid bed catalyst reactor is allowed to cool to room temperature.

[0013] Preferably, the catalyst in step D is a composite DMDS vulcanizing agent.

[0014] Preferably, the temperature in step C is 150 degrees Celsius.

[0015] Preferably, the inert gas in step B is nitrogen, and the nitrogen is introduced for 1 hour.

[0016] Preferably, in step D, the sulfiding agent is injected in sections, with each section injecting for 10 to 30 minutes, and the time interval between two adjacent injection sections is 5 to 15 minutes.

[0017] Preferably, in step C, during the preheating process, the temperature rise curve inside the solid bed catalyst reactor is stepped, first heating to 100 degrees Celsius at a rate of 10 degrees Celsius per hour to 15 degrees Celsius per hour, maintaining for 1 to 2 hours, and then heating to the target temperature at a rate of 15 degrees Celsius per hour to 20 degrees Celsius per hour.

[0018] Preferably, in step E, the amount of cold hydrogen introduced is adjusted in real time according to the temperature of the catalyst bed. When the temperature exceeds 380 degrees Celsius, the amount of cold hydrogen introduced is increased by 10% to 20%, and when the temperature is lower than 320 degrees Celsius, the amount of cold hydrogen introduced is reduced by 5% to 10%.

[0019] Compared with the prior art, the advantages of the present invention are:

[0020] 1. This solution uses a composite DMDS vulcanizing agent as the vulcanizing agent. The composite DMDS vulcanizing agent has an initial vulcanization temperature below 150°C, high vulcanization efficiency, and a small temperature rise during the vulcanization process. Furthermore, the composite DMDS vulcanizing agent offers advantages such as low odor, a high flash point, and vulcanization safety. Combined with vulcanization process optimization, this significantly shortens the vulcanization time and ensures that the hydrogen sulfide content in the hydrogenation unit reaction system meets or exceeds the design standard of 200 ppm. Furthermore, the introduction of cooling air prevents a sharp increase in the catalyst bed temperature and avoids a decrease in catalyst activity due to sintering, thereby saving vulcanization time and protecting the catalyst.

[0021] Second, by injecting the sulfiding agent in stages, the sulfiding agent can be fully in contact with the catalyst, further improving the sulfiding efficiency. At the same time, it avoids the catalyst bed temperature being too high due to the one-time injection of a large amount of sulfiding agent, thereby better protecting the activity of the catalyst. This step-by-step heating method can make the catalyst bed evenly heated, reduce the internal stress concentration of the catalyst caused by excessive temperature gradient, and thus reduce the risk of damage to the catalyst bed structure and extend the service life of the catalyst. DETAILED DESCRIPTION

[0022] Example 1:

[0023] An industrial-grade grease catalyst vulcanization process comprises the following steps:

[0024] A. Select an industrial grease catalyst, select a mixture of molybdenum trioxide and nickel oxide as the catalyst, and add the catalyst into a solid bed catalyst reactor to form a catalyst bed.

[0025] B. Exhaust air: Use nitrogen in the inert gas to pass into the solid bed catalyst reactor. The purge time is one hour to purge the catalyst bed and exclude air to avoid side reactions between the catalyst bed and air under the action of high temperature.

[0026] C. Catalyst preheating: The internal catalyst bed is preheated by the heating equipment of the solid bed catalyst reactor itself. The temperature range is controlled at 150 degrees Celsius, and the heating rate is 20 degrees Celsius per hour. During the preheating process, the temperature rise curve inside the solid bed catalyst reactor is step-shaped, first heating to 100 degrees Celsius at a rate of 15 degrees Celsius per hour, maintaining for 1 hour, and then heating to 150 degrees Celsius at a rate of 20 degrees Celsius per hour. This step-by-step heating method can make the catalyst bed evenly heated, reduce the internal stress concentration of the catalyst caused by excessive temperature gradient, thereby reducing the risk of damage to the catalyst bed structure and extending the service life of the catalyst.

[0027] D. Select a vulcanizing agent, select a composite DMDS vulcanizing agent as the vulcanizing agent, introduce the vulcanizing agent into the interior of the fixed-bed catalyst reactor, control the injection pressure of the vulcanizing agent at 1 MPa, control the pressure inside the solid-bed catalyst reactor at 10 MPa, and inject the vulcanizing agent in a segmented manner, with each segment injection time being 25 minutes and the interval between two adjacent injection segments being 5 minutes. By injecting the vulcanizing agent in segments, the vulcanizing agent can be fully contacted with the catalyst, further improving the vulcanization efficiency and avoiding excessively high catalyst bed temperature due to the one-time injection of a large amount of vulcanizing agent, thereby better protecting the activity of the catalyst;

[0028] E. At the beginning of step D, cold hydrogen is introduced into the solid bed catalyst reactor. The amount of cold hydrogen introduced is adjusted in real time according to the temperature of the catalyst bed. When the temperature exceeds 380 degrees Celsius, the amount of cold hydrogen introduced is increased by 20%. When the temperature is lower than 320 degrees Celsius, the amount of cold hydrogen introduced is reduced by 5%. The temperature of the catalyst bed is monitored by a temperature sensor inside the solid bed catalyst reactor to maintain the temperature between 350 degrees Celsius.

[0029] F. After the sulfurization is completed, the injection of the sulfurizing agent is stopped and the catalyst bed inside the solid bed catalyst reactor is allowed to cool to room temperature.

[0030] Example 2:

[0031] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 1 is that the initial temperature of the vulcanizing agent in step C of Example 2 is controlled at 250 degrees. The other conditions are exactly the same as those in Example 1. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0032] Example 3:

[0033] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 1 is that the initial temperature of the vulcanizing agent in step C of Example 3 is controlled at 350 degrees. The other conditions are exactly the same as those in Example 1. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0034] Example 4:

[0035] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 1 is that dimethyl disulfide (DMDS) is used as the vulcanizing agent in Step D of Example 4. The remaining conditions are identical to those of Example 1. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0036] Example 5:

[0037] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 4 is that the initial temperature of the vulcanizing agent in step D of Example 5 is controlled at 250 degrees Celsius. The remaining conditions are identical to those of Example 4. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0038] Example 6:

[0039] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 4 is that the initial temperature of the vulcanizing agent in Step D of Example 6 is controlled at 350 degrees Celsius. The remaining conditions are identical to those of Example 4. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0040] Example 7:

[0041] An industrial-grade grease catalyst vulcanization process is described. The difference from Example 1 is that carbon disulfide (CS2) is used as the vulcanizing agent in Step D of Example 7. The remaining conditions are identical to those of Example 1. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0042] Example 8:

[0043] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 7 is that the initial temperature of the vulcanizing agent in step D of Example 8 is controlled at 250 degrees. The remaining conditions are identical to those of Example 7. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0044] Example 9:

[0045] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 7 is that the initial temperature of the vulcanizing agent in Step D of Example 9 is controlled at 350 degrees Celsius. The remaining conditions are identical to those of Example 7. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0046] Example 10:

[0047] An industrial-grade grease catalyst vulcanization process is described. The difference from Example 1 is that dimethyl sulfide (DMS) is used as the vulcanizing agent in Step D of Example 10. The remaining conditions are identical to those of Example 1. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0048] Example 11:

[0049] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 10 is that the initial temperature of the vulcanizing agent in Step D of Example 11 is controlled at 250 degrees. The other conditions are exactly the same as those in Example 10. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0050] Example 12:

[0051] An industrial-grade grease catalyst vulcanization process is provided. The difference from Example 10 is that the initial temperature of the vulcanizing agent in Step D of Example 12 is controlled at 350 degrees Celsius. The remaining conditions are identical to those of Example 10. The vulcanization time, the amount of cold hydrogen added, and the hydrogen sulfide content of the product are recorded.

[0052]

[0053]

[0054] A composite DMDS vulcanizing agent is used as the catalyst's vulcanizing agent. The initial vulcanization temperature of the composite DMDS vulcanizing agent is below 150°C, resulting in high vulcanization efficiency. The small amount of cold hydrogen required means a small temperature rise during the vulcanization process. Furthermore, the composite DMDS vulcanizing agent itself has advantages such as low odor, high flash point, and vulcanization safety. Combined with the optimization of the vulcanization process, the vulcanization time is significantly shortened, ensuring that the hydrogen sulfide content in the hydrogenation unit reaction system reaches or exceeds the design standard of 200ppm. The cold hydrogen introduction step also prevents a sharp increase in the catalyst bed temperature and avoids a decrease in catalyst activity due to sintering, thereby saving vulcanization time and protecting the catalyst.

Claims

1. An industrial-grade grease catalyst vulcanization process, characterized by: The following steps are involved: A. Select an industrial grease catalyst, select a mixture of molybdenum trioxide and nickel oxide as a catalyst, and add the catalyst into a solid bed catalyst reactor to form a catalyst bed; B. Exhaust air: use inert gas to pass into the solid bed catalyst reactor to purge the catalyst bed and remove air; C. Catalyst preheating: The catalyst bed inside the solid bed catalyst reactor is preheated by the heating equipment of the solid bed catalyst reactor itself. The temperature range is controlled between 100 degrees Celsius and 400 degrees Celsius, and the heating rate is between 10 degrees Celsius per hour and 30 degrees Celsius per hour; D. Select a vulcanizing agent, select one or more of dimethyl disulfide (DMDS), carbon disulfide (CS2), dimethyl sulfide (DMS) and a composite DMDS vulcanizing agent as the vulcanizing agent, introduce the vulcanizing agent into the interior of the fixed bed catalyst reactor, control the injection pressure of the vulcanizing agent to be between 1 MPa and 2 MPa, and control the pressure inside the solid bed catalyst reactor to be between 1 MPa and 10 MPa; E. At the beginning of step D, cold hydrogen is introduced into the solid bed catalyst reactor, and the temperature of the catalyst bed is monitored by a temperature sensor inside the solid bed catalyst reactor to maintain the temperature between 100 degrees Celsius and 400 degrees Celsius; F. After the sulfurization is completed, the injection of the sulfurizing agent is stopped and the catalyst bed inside the solid bed catalyst reactor is allowed to cool to room temperature.

2. The industrial-grade grease catalyst vulcanization process according to claim 1, characterized in that: The vulcanizing agent in step D is a composite DMDS vulcanizing agent.

3. An industrial-grade grease catalyst vulcanization process according to claim 2, characterized in that: The temperature in step C is 150 degrees Celsius.

4. The industrial-grade grease catalyst vulcanization process according to claim 1, characterized in that: The inert gas in step B is nitrogen, and the nitrogen is introduced for 1 hour.

5. The industrial-grade grease catalyst vulcanization process according to claim 1, characterized in that: In the step D, the sulfiding agent is injected in sections, with each section injecting for 10 to 30 minutes, and the time interval between two adjacent injection sections is 5 to 15 minutes.

6. The industrial-grade grease catalyst vulcanization process according to claim 1, characterized in that: In step C, during the preheating process, the temperature rise curve inside the solid bed catalyst reactor is step-shaped, firstly heating to 100 degrees Celsius at a rate of 10 degrees Celsius per hour to 15 degrees Celsius per hour, maintaining for 1 to 2 hours, and then heating to the target temperature at a rate of 15 degrees Celsius per hour to 20 degrees Celsius per hour.

7. The industrial-grade grease catalyst vulcanization process according to claim 1, characterized in that: In step E, the amount of cold hydrogen introduced is adjusted in real time according to the temperature of the catalyst bed. When the temperature exceeds 380 degrees Celsius, the amount of cold hydrogen introduced is increased by 10% to 20%. When the temperature is lower than 320 degrees Celsius, the amount of cold hydrogen introduced is reduced by 5% to 10%.

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