CN110373227B - Hydrogenation reaction method and device for inhibiting coking under hydrogen atmosphere protection - Google Patents
Hydrogenation reaction method and device for inhibiting coking under hydrogen atmosphere protection Download PDFInfo
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- CN110373227B CN110373227B CN201910598179.8A CN201910598179A CN110373227B CN 110373227 B CN110373227 B CN 110373227B CN 201910598179 A CN201910598179 A CN 201910598179A CN 110373227 B CN110373227 B CN 110373227B
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
- C10G65/14—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural parallel stages only
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Abstract
A hydrogenation reaction method and a device for inhibiting coking by hydrogen atmosphere protection are provided, wherein hydrogen is divided into four branches to respectively contact and react with an oil product. Premixing a first part of hydrogen and raw oil in a vortex mixer; injecting a second part of hydrogen into the bottom of the hydrogenation reactor, and allowing the hydrogen and the raw oil to enter a homogeneous bubble shearing member; a third portion of the hydrogen gas is injected into the mesoscale bubble generation member; the fourth portion of hydrogen gas is injected as cold hydrogen into the cold hydrogen opening member. Through the adjustment of the hydrogen concentration distribution of the main part, the coking caused by local hydrogen lack is avoided, the hydrogenation conversion rate is improved, and the continuous operation period of residual oil hydrogenation is prolonged.
Description
Technical Field
The invention relates to a hydrogenation reaction method and a device for inhibiting coking by hydrogen atmosphere protection, in particular to a method and a device for improving the hydrogen homogeneity of oil, further improving the hydrogenation conversion rate and avoiding coking by utilizing a full-process hydrogen atmosphere protection method and a full-process hydrogen atmosphere protection device aiming at the difficult problem of easy coking of poor oil hydrogenation reaction such as heavy oil, residual oil and the like, and is suitable for the hydrogenation process of a fixed bed, a fluidized bed and a slurry bed.
Background
Petroleum resources are non-renewable resources and are the main energy and chemical raw material sources on which human beings rely for survival at present. With the increasing shortage of petroleum resources, the processing proportion of heavy crude oil will be larger and larger, so the selection of heavy oil processing schemes influences the economic benefit and even fate of refineries.
The residua is typically divided into four components: saturates, aromas, gums, and asphaltenes. The stability of the residuum colloid system depends on the composition and structure of the residuum system and changes in external conditions, such as heat treatment temperature and residence time, which affect the phase separation characteristics of the residuum system by changing the composition and structure of the residuum. In the residual oil system, asphaltenes and colloid heavy components form mixed micelles, which are the main factors of coking.
In the hydrogenation reaction process, hydrocracking is an aromatic ring breaking process, the proportion of heavy solvent components for dissolving asphaltene is reduced, and the aromaticity is reduced due to hydrogenation saturation, the asphaltene is separated out due to supersaturation and becomes a precursor of coking, and the asphaltene is separated out at the following high-temperature parts to cause the reduction of the operation performance of the device: the reactor, the interstage knockout drum, the hot low-pressure knockout drum, the hot medium-pressure knockout drum, the atmospheric tower bottom, the vacuum furnace, the vacuum tower bottom and the bottom-reducing heat exchanger, etc., influence the economic benefits of the whole plant or shorten the operation cycle of the device.
The Chevron company VRSH process uses a strong hydrogenation type homogeneous catalyst to improve hydrogenation activity and inhibit coke formation. The EST process of Eni company and the Uniflex technology of UOP company adopt temperature to control reaction conversion rate so as to control coke formation limit, but have the problems of high cost, complex operation and the like.
In the residue hydrocracking process, the decrease of hydrogen partial pressure leads to the increase of precipitates in reaction products (refer to the research of anti-coking technology of the ebullated bed oil plus ammonia cracking device, Wuhan engineering university, Master's academic paper). The hydrogen partial pressure at a certain position in the reactor is equal to the pressure of the reactor multiplied by the hydrogen concentration, and the increase of the hydrogen partial pressure can inhibit the coking reaction and reduce the catalyst deactivation rate on one hand; on the other hand, the removal rate of sulfur, nitrogen and metal can be improved, and meanwhile, the hydrogenation saturation reaction of the polycyclic aromatic hydrocarbon can be promoted. The hydrogen partial pressure can not be continuously increased, and the release of reaction heat and the consumption of ammonia are increased while the hydrogen partial pressure is increased, so that the temperature difference between the outlet and the inlet of the catalyst bed is increased, and the service life and the operation of the catalyst in the reactor are adversely affected.
Microscopically, the hydrogen concentration at certain locations of the hydrogenation reactor is not effectively controlled, resulting in coking during thermal cracking. Meanwhile, the coking speed is increased along with the increase of the reaction temperature and the conversion rate, the conversion rate of products is usually artificially limited for long-period operation, and the hydrogenation conversion rate is limited by coking.
Disclosure of Invention
The invention aims to improve the hydrogen atmosphere protection level in the whole reaction process by accurately adjusting the concentration distribution of hydrogen in the reactor, and is a method for effectively inhibiting coking and improving the conversion rate.
The specific technical scheme of the invention is as follows:
a hydrogenation reaction method for inhibiting coking under hydrogen atmosphere protection comprises the following steps that hydrogen is divided into four branches to be respectively in contact reaction with an oil product, and the first part of hydrogen and raw oil are premixed in a vortex mixer; injecting a second part of hydrogen into the bottom of the hydrogenation reactor, and allowing the hydrogen and the raw oil to enter a homogeneous bubble shearing member; a third portion of the hydrogen gas is injected into the mesoscale bubble generation member; the fourth portion of hydrogen gas is injected as cold hydrogen into the cold hydrogen opening member.
Hydrogen is quickly dissolved in the raw oil in the premixing process, the premixed hydrogen exists in liquid-phase raw oil in a dissolved form and a micro-bubble form, and the volume flow ratio of the premixed hydrogen to the raw oil is 5-30% under the working condition;
an annular bubbling member and a vortex shearing member are arranged in the vortex mixer, the raw oil handling capacity of a single vortex shearing member is 4-9 square meters per hour, and the pressure drop of hydrogen and raw oil in the premixing process is not more than 3.5 bar;
the volume flow ratio range of the hydrogen injected into the bottom of the hydrogenation reactor under the working condition to the raw oil is 0-120%, and bubbles with the size of 1-1000 microns are formed in the homogeneous bubble shearing component;
the homogeneous bubble shearing component adopts a rotational flow shearing and jet coupling structure type, and the raw oil handling capacity of a single homogeneous bubble shearing component is 2-6 square per hour;
calculating the hydrogen flow injected into the mesoscale bubble generating component under the working condition according to the hydrogen airspeed of the hydrogenation reactor, and closing the liquid-phase circulating pump of the process, wherein the size of the formed hydrogen bubbles is 0.1-30 mm;
hydrogen injected into the mesoscale bubble generation component can be mixed with part of the extracted liquid phase and injected, at the moment, a liquid phase circulating pump of the process is started, and the size of the formed hydrogen bubbles is 0.1-10 mm;
the hydrogen flow rate of the cold hydrogen open pore component injected under the working condition is calculated according to the hydrogenation temperature rise control, the liquid phase circulating pump of the process is closed, and the size of the formed bubbles is 2-30 mm;
the hydrogen injected into the cold hydrogen open pore component can be mixed with part of the extracted liquid phase for injection, the liquid phase circulating pump of the process is opened at the moment, and the size of the formed hydrogen bubbles is 0.1-10 mm.
A hydrogenation reaction device with hydrogen atmosphere protection and coking inhibition mainly comprises a vortex mixer, a homogeneous bubble shearing component, a mesoscale bubble generating component and a cold hydrogen pore-forming component.
An annular bubbling member and a vortex shearing member are arranged in the vortex mixer, a circular hole with the diameter of 3-8 mm is formed in the annular bubbling member, the vortex shearing member is installed in parallel on a cavity partition plate, and the vortex shearing member guides the vortex flow through a spiral blade to realize hydrogen crushing and hydrogen dissolution;
the homogeneous bubble shearing component is arranged on the lower convex clapboard in parallel, and the ratio of the height difference of the highest and lowest positions of the lower convex clapboard to the diameter of the reactor is 0.01-0.3;
the structure type of the mesoscale bubble generation component comprises a disc opening hole, a pipe opening hole and a bubble cap, and the height difference between the mesoscale bubble generation component and the homogeneous bubble shearing component is 100-500 mm;
the structural style of the cold hydrogen open pore member comprises a disk open pore, a pipe open pore and a bubble cap, wherein the cold hydrogen open pore member can be a plurality of open pores with the size not less than 5mm on the height of the reactor;
in another embodiment, 1-10 holes with the diameter of 5mm are formed in the lower position of the lower convex partition plate, so that the reactor stops working and returns materials thoroughly;
in another embodiment, no hydrogen is injected into the bottom of the hydrogenation reactor, and all the hydrogen entering the homogeneous bubble shearing component together with the raw oil is premixed hydrogen;
the invention provides a process method for inhibiting coking by hydrogen atmosphere protection aiming at the difficult problem of hydrogenation coking, which homogenizes the hydrogen concentration of the whole reaction area by utilizing the adjustment of a hydrogen feeding mode, can properly heat up to improve the hydrogenation conversion rate on the premise of inhibiting coking, and prolongs the running period of the device.
The invention has the beneficial effects that:
(1) through the adjustment of the hydrogen concentration distribution of the main part, the condition of local hydrogen lack is avoided, the coking rate is inhibited, and the improvement of the hydrogenation conversion rate is promoted.
(2) The temperature distribution of the slurry bed is more uniform, the phenomenon of local coking is inhibited, and the continuous operation period of residual oil hydrogenation is prolonged.
(3) The core component is a static component, the size of the flow channel is large, the structure is simple, and the operation is simple and easy.
Drawings
FIG. 1 is a schematic diagram of an apparatus for upflow hydrogenation;
FIG. 2 is a schematic view of a premixing process vortex mixer;
FIG. 3 is a schematic view of a homogenizing bubble shear member;
description of the symbols:
1, a vortex mixer, 2 homogeneous bubble shearing components, 3 mesoscale bubble generating components, 4 cold hydrogen tapping components, 5 first liquid phase circulating pumps and 6 second liquid phase circulating pumps;
1-1 vortex mixer liquid phase inlet; 1-2 vortex mixer reactor annular bubbling member;
1-3 vortex shear elements of a vortex mixer; 1-4 vortex mixer cavity baffles;
1-5 liquid phase inlets of a vortex mixer; 1-6 vortex mixer mixing back cavity;
1-7 vortex mixer mixing front cavity; 1-8 vortex mixer hydrogen inlet;
2-1 homogenizing bubble shearing component inlet distribution cavity; 2-2 a homogeneous bubble shear member spacer;
2-3 a homogeneous bubble shear member; 2-4 homogenizing bubble shearing member outlet cavity.
Detailed Description
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the invention by those skilled in the art based on the teachings herein are within the scope of the present invention.
As shown in FIG. 1, the hydrogenation reaction device with hydrogen atmosphere protection and coking inhibition comprises a vortex mixer 1, a homogeneous bubble shearing component 2, a mesoscale bubble generation component 3 and a cold hydrogen pore-forming component 4; an annular bubbling member and a vortex shearing member are arranged in the vortex mixer, a circular hole with the diameter of 3-8 mm is formed in the annular bubbling member, the vortex shearing member is arranged on a cavity partition plate in parallel, and the vortex shearing member guides a vortex flow through a spiral blade to realize hydrogen crushing and hydrogen dissolution; the homogeneous bubble shearing component is arranged on the lower convex clapboard in parallel, and the ratio of the height difference of the highest and lowest positions of the lower convex clapboard to the diameter of the reactor is 0.01-0.3.
FIG. 2 is a schematic view of a premixing process vortex mixer; the device is a premixing process vortex mixer, wherein two ends of the premixing process vortex mixer are respectively provided with a vortex mixer liquid phase inlet 1-1 and a vortex mixer liquid phase inlet 1-5, the middle part of the premixing process vortex mixer is provided with a vortex mixer cavity partition plate 1-4 which is divided into a vortex mixer mixing rear cavity 1-6 and a vortex mixer mixing front cavity 1-7, a vortex mixer reactor annular bubbling component 1-2 connected with a vortex mixer hydrogen inlet 1-8 is arranged in the front cavity 1-7, and a vortex mixer vortex shearing component 1-3 is arranged on the cavity partition plate and is installed in parallel.
FIG. 3 is a schematic view of a homogeneous bubble shear member; the homogenizing bubble shearing component 2-2 is divided into a homogenizing bubble shearing component inlet distribution cavity 2-1 and a homogenizing bubble shearing component outlet 2-4, and the homogenizing bubble shearing component 2-3 is arranged on the partition plate.
The hydrogen is divided into four branches which are respectively in contact reaction with oil products, and the first part of hydrogen and the raw oil are premixed in a vortex mixer; injecting a second part of hydrogen into the bottom of the hydrogenation reactor, and allowing the hydrogen and the raw oil to enter a homogeneous bubble shearing member; a third portion of the hydrogen gas is injected into the mesoscale bubble generation member; the fourth portion of hydrogen gas is injected as cold hydrogen into the cold hydrogen opening member.
Calculating the hydrogen flow injected into the mesoscale bubble generating component under the working condition according to the hydrogen airspeed of the hydrogenation reactor, and closing the liquid-phase circulating pump 5 of the process, wherein the size of the formed hydrogen bubbles is 0.1-30 mm; hydrogen injected into the mesoscale bubble generation component and part of the extracted liquid phase are mixed and injected under the working condition, at the moment, a liquid phase circulating pump 5 of the process is started, and the size of the formed hydrogen bubbles is 0.1-10 mm; the hydrogen flow rate of the cold hydrogen open pore component injected under the working condition is calculated according to the hydrogenation temperature rise control, the liquid phase circulating pump 6 of the process is closed, and the size of the formed bubbles is 2-30 mm; the hydrogen of cold hydrogen trompil component is injected under the operating mode can mix with the liquid phase of part extraction and pour into, opens the liquid phase circulating pump 6 of this flow this moment, and the hydrogen bubble size of formation is 0.1 ~ 10 millimeters.
Example 1
In a fixed bed residual oil hydrogenation process of a petrochemical plant, carbon residue and conversion rate measurements are performed before and after a hydrogen atmosphere protection method is adopted, and are shown in the following table.
| Before hydrogen atmosphere protection method | After the hydrogen atmosphere protection method | |
| Residual oil raw material carbon residue, wt% | 11 | 11.3 |
| Carbon residue of the product wt% | 5.9 | 5 |
| Product precipitate, wt% | 0.8 | 0.3 |
| Conversion rate | 60 | 75 |
When the method and the device are used for carrying out residual oil hydrogenation on the fixed bed, the product sediment is reduced to 0.3 percent from the original 0.8 percent, and the conversion rate is improved to 75 percent from the original 60 percent.
The main advantages of the invention are:
according to the invention, on the basis of the traditional hydrogenation reactor, the hydrogen injection form is accurately controlled, hydrogen atmosphere protection is formed in the whole reaction area, coking caused by local hydrogen deficiency is avoided, the conversion rate of residual oil hydrogenation reaction is improved, the effective utilization rate of hydrogen is improved, and the economic benefit is obvious.
Claims (7)
1. A hydrogenation reaction method for inhibiting coking under hydrogen atmosphere protection, hydrogen is divided into four branches to respectively contact and react with an oil product, and is characterized in that the first part of hydrogen and raw oil are premixed in a vortex mixer; injecting a second part of hydrogen into the bottom of the hydrogenation reactor, and allowing the hydrogen and the raw oil to enter a homogeneous bubble shearing member; a third portion of the hydrogen gas is injected into the mesoscale bubble generation member; injecting the fourth part of hydrogen as cold hydrogen into the cold hydrogen open pore component; wherein:
hydrogen is quickly dissolved in the raw oil in the premixing process, the premixed hydrogen exists in liquid-phase raw oil in a dissolved form and a micro-bubble form, and the volume flow ratio of the premixed hydrogen to the raw oil is 5-30% under the working condition;
hydrogen injected into the bottom of the hydrogenation reactor forms bubbles with the size of 1-1000 microns in the homogeneous bubble shearing component, and the volume flow ratio range of the hydrogen injected into the bottom of the hydrogenation reactor to the raw oil under the working condition is 0-120% but not 0;
calculating the hydrogen flow injected into the mesoscale bubble generating component under the working condition according to the hydrogen airspeed of the hydrogenation reactor, and closing the liquid-phase circulating pump of the process, wherein the size of the formed hydrogen bubbles is 0.1-30 mm; hydrogen injected into the mesoscale bubble generation component and part of the extracted liquid phase are mixed and injected under the working condition, at the moment, a liquid phase circulating pump of the process is started, and the size of the formed hydrogen bubbles is 0.1-10 mm;
the hydrogen flow rate of the cold hydrogen open pore component injected under the working condition is calculated according to the hydrogenation temperature rise control, the liquid phase circulating pump of the process is closed, and the size of the formed bubbles is 2-30 mm; the hydrogen of cold hydrogen trompil component is injected into under the operating mode and the liquid phase of part extraction is mixed and is injected, opens the liquid phase circulating pump of this flow this moment, and the hydrogen bubble size of formation is 0.1 ~ 10 millimeters.
2. The method according to claim 1, wherein the vortex mixer is internally provided with an annular bubbling member and a vortex shearing member, the processing amount of raw oil of a single vortex shearing member is 4-9 square per hour, and the pressure drop of hydrogen and raw oil in the premixing process is not more than 3.5 bar.
3. The method according to claim 1, wherein the homogeneous bubble shearing component adopts a rotational flow shearing and jet coupling structure type, and the raw oil handling capacity of a single homogeneous bubble shearing component is 2-6 squares per hour.
4. The method according to claim 1, wherein an annular bubbling member and a vortex shearing member are arranged in the vortex mixer, the annular bubbling member is provided with a circular hole with the diameter of 3-8 mm, the vortex shearing member is arranged in parallel on a cavity partition plate, and the vortex shearing member guides the rotational flow through a spiral blade to realize hydrogen crushing and hydrogen dissolution; the homogeneous bubble shearing component is arranged on the lower convex clapboard in parallel, and the ratio of the height difference of the highest and lowest positions of the lower convex clapboard to the diameter of the reactor is 0.01-0.3.
5. The method according to claim 4, wherein the difference in height between the mesoscale bubble generation means and the homogeneous bubble shearing means is 100 to 500 mm.
6. The method of claim 4, wherein the cold hydrogen vent structure is provided in plurality over the height of the reactor with a vent size of not less than 5 mm.
7. The method as claimed in claim 4, wherein the lower position of the lower convex clapboard is provided with 1-10 holes with the diameter of 5mm, so that the reactor is shut down and completely returned.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101410171A (en) * | 2006-03-31 | 2009-04-15 | 布莱尔·H·希尔斯 | Apparatus for mixing gasses and liquids |
| CN105647577A (en) * | 2014-11-13 | 2016-06-08 | 中国石油天然气股份有限公司 | Continuous liquid phase hydrogenation process and device for hydrocarbons |
| CN107952401A (en) * | 2016-10-17 | 2018-04-24 | 北京华石联合能源科技发展有限公司 | A kind of floating bed hydrogenation cold wall reactor |
| CN108203599A (en) * | 2016-12-16 | 2018-06-26 | 中国石油天然气股份有限公司 | Method for removing aromatic hydrocarbon from synthetic oil |
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2019
- 2019-07-04 CN CN201910598179.8A patent/CN110373227B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101410171A (en) * | 2006-03-31 | 2009-04-15 | 布莱尔·H·希尔斯 | Apparatus for mixing gasses and liquids |
| CN105647577A (en) * | 2014-11-13 | 2016-06-08 | 中国石油天然气股份有限公司 | Continuous liquid phase hydrogenation process and device for hydrocarbons |
| CN107952401A (en) * | 2016-10-17 | 2018-04-24 | 北京华石联合能源科技发展有限公司 | A kind of floating bed hydrogenation cold wall reactor |
| CN108203599A (en) * | 2016-12-16 | 2018-06-26 | 中国石油天然气股份有限公司 | Method for removing aromatic hydrocarbon from synthetic oil |
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Effective date of registration: 20220810 Address after: 201514 room 3533, building 1, No. 2758, Songjin Road, Zhangyan Town, Jinshan District, Shanghai Patentee after: SHANGHAI MISU ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Patentee after: Ji'an Yonglan (Beijing) Engineering Technology Development Co.,Ltd. Patentee after: SINOPEC ENGINEERING Inc. Address before: 201514 room a3533, building 1, 2758 Songjin Road, Zhangyan Town, Jinshan District, Shanghai Patentee before: SHANGHAI MISU ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Patentee before: Ji'an Yonglan (Beijing) Engineering Technology Development Co.,Ltd. |
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