CN112111295A - Low-temperature pyrolysis method and system for residual oil hydrogenation waste catalyst - Google Patents
Low-temperature pyrolysis method and system for residual oil hydrogenation waste catalyst Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
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- C—CHEMISTRY; METALLURGY
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
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Abstract
The invention discloses a low-temperature pyrolysis method and a system for residual oil hydrogenation spent catalyst, wherein the method comprises the following steps: s100, deoiling the raw materials; s200, primary oil is gasified; s300, gasifying secondary oil; s400, collecting materials; s500, liquid oil recovery, all processes of feeding, discharging, liquid oil recovery, oil gas self-circulation and the like of the invention realize automatic, continuous and industrialized operation, the whole process does not need to change operating places, unnecessary heat loss can be effectively prevented, the electric energy consumption can be reduced, the pressure and the temperature of the first rotary kiln and the second rotary kiln can be accurately controlled, the oil content of the raw materials can be deoiled for multiple times and repeatedly until the oil content is completely and thoroughly treated, the invention has no harmful tail gas emission, is beneficial to environmental protection, can recover a large amount of liquid oil, does not need to add any reagent, can save a large amount of funds, thoroughly avoids the generation of new impurities, and achieves multiple purposes.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a low-temperature pyrolysis method and a low-temperature pyrolysis system for a residual oil hydrogenation waste catalyst.
Background
In the prior art, no particularly effective treatment method exists for the residual oil hydrogenation spent catalyst at present, the existing treatment method is generally a simple heating treatment, the treatment equipment is generally a heating reaction kettle, and the existing residual oil hydrogenation spent catalyst treatment technology at least has the following technical defects:
1. during heating treatment, oil is gasified, so that the pressure in the reaction kettle is quickly increased, the reaction is slowed down and even stopped, and the sealing performance of the reaction kettle is reduced;
2. during heating treatment, oil is gasified, so that the concentration of oil and gas in a reaction kettle is increased suddenly, the gasification temperature is increased, the volatilization efficiency of the oil and gas is slowed, more heat energy (electric heating) is needed for oil gasification, and the production cost is greatly increased;
3. during heating treatment, the oil content gasification condition is unstable, so that the technological parameters such as temperature, pressure and the like in a reaction kettle cannot be accurately controlled, the oil content cannot be completely and thoroughly treated, and continuous production cannot be realized;
4. during heating treatment, discharged oil gas cannot be cooled in time, a large amount of liquid oil contained in the oil gas cannot be effectively recovered, the oil gas is directly discharged to pollute the environment, and a large amount of capital investment is required during oil gas purification treatment;
5. during the heating process, can only intermittent type formula heating process, a batch material has been handled and has been cooled down, discharges and carries out next batch to need the cooperation of a plurality of reation kettle to use, the frequent switching operation place of raw materials not only wastes time and energy, has occupied a large amount of operating space, but also leads to the production incident easily.
6. During heating treatment, temperature rise and temperature reduction are required frequently, energy consumption is high, treatment capacity is low, a large amount of manpower and material resources are wasted, and automatic, large-batch and industrial operation is difficult to perform.
Therefore, it is urgent and significant to find an effective low-temperature pyrolysis method and system for residual oil hydrogenation spent catalyst.
Disclosure of Invention
The present invention is directed to a method and system for low temperature pyrolysis of a residual oil hydrogenation catalyst to solve the above problems of the prior art.
In one aspect, the invention discloses a low temperature pyrolysis method of residual oil hydrogenation spent catalyst, which comprises the following steps:
s100, deoiling raw materials: the raw materials are sequentially subjected to deoiling through a first rotary kiln (2) and a second rotary kiln (3) by using a feeding screw conveyor (1);
s200, primary oil gasification: the temperature in the first rotary kiln (2) is 300-;
s300, secondary oil gasification: the temperature in the second rotary kiln (3) is 300-;
s400, collecting materials: the solid materials after deoiling leave the feeding screw conveyor (1) and enter a kiln tail sealing cover (4), then fall from the kiln tail sealing cover (4) and enter a discharging screw conveyor (5), a cooling water inlet pipe (6) and a cooling water outlet pipe (7) are communicated with cold water, and the solid materials fall into a material receiving barrel (8) after being cooled;
s500, liquid oil recovery: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9) and an oil-water separator (10), are cooled into liquid oil and then enter an oil tank (11) for recovery;
s600, oil gas self-circulation: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9), an oil-water separator (10) and a heat exchanger (21) to form liquid oil and non-condensable gas, the liquid oil enters an oil tank (11) to be recovered, the non-condensable gas sequentially passes through a water seal flame-retardant tank (12), a water ring vacuum pump (13), a circulating water tank (14), a tail gas pipeline (15) and a tail gas water seal tank (16) and then enters a kiln tail sealing cover (4) and a kiln head sealing cover (17), and the oil gas in the furnace is blown out of a hearth to form an oil gas self-circulation passage.
According to the embodiment of the invention, in step S600, liquid oil is formed when the non-condensable gas passes through the water-sealed flame-retardant tank (12), and the liquid oil enters the oil tank (11) for recovery.
According to an embodiment of the invention, the first rotary kiln (2) and the second rotary kiln (3) are sealed external heating rotary furnaces.
According to an embodiment of the invention, the first rotary kiln (2) and the second rotary kiln (3) are rotated at 20 hz.
According to an embodiment of the invention, the feed screw (1) rotates at 2-5 Hz and the discharge screw (5) rotates at 3-10 Hz.
According to an embodiment of the invention, the time for de-oiling the raw material in the first rotary kiln (2) and the second rotary kiln (3) is 3 hours.
In another aspect, the present invention also discloses a system suitable for the low temperature pyrolysis method of the residual oil hydrogenation spent catalyst, which comprises: the device comprises a feeding spiral conveyor (1), a first rotary kiln (2), a second rotary kiln (3), a kiln tail sealing cover (4), a discharging spiral conveyor (5), a cooling water inlet pipe (6), a cooling water outlet pipe (7), a receiving barrel (8), a surface cooling pipeline (9), an oil-water separator (10), an oil tank (11), a water-seal flame-retardant tank (12), a water ring vacuum pump (13), a circulating water tank (14), a tail gas pipeline (15), a kiln head sealing cover (17), an oil-gas pipeline (18) and a heat exchanger (21);
the feeding screw conveyor (1) penetrates through the first rotary kiln (2) and the second rotary kiln (3) so as to convey raw materials to sequentially pass through the first rotary kiln (2) and the second rotary kiln (3) for deoiling respectively;
the first rotary kiln (2) is connected with the kiln head sealing cover (17), the second rotary kiln (3) is connected with the kiln tail sealing cover (4), the kiln head sealing cover (17) and the kiln tail sealing cover (4) are both connected with the oil-gas pipeline (18), the surface cooling pipeline (9) is connected with the oil-gas pipeline (18), the oil-water separator (10) is connected with the surface cooling pipeline (9), and the oil tank (11) is connected with the oil-water separator (10);
the heat exchanger (21) is respectively connected with the oil-water separator (10) and the oil tank (11), the water-sealed flame-retardant tank (12) is connected with the heat exchanger (21), the water-ring vacuum pump (13) is connected with the water-sealed flame-retardant tank (12), the circulating water tank (14) is connected with the water-ring vacuum pump (13), the tail gas pipeline (15) is connected with the circulating water tank (14), and the kiln head sealing cover (17) and the kiln tail sealing cover (4) are both connected with the tail gas pipeline (15);
the discharging screw conveyor (5) is connected with the kiln tail sealing cover (4), the cooling water inlet pipe (6) and the cooling water outlet pipe (7) are both connected with the discharging screw conveyor (5), and the receiving barrel (8) is arranged below the discharging screw conveyor (5).
According to the embodiment of the invention, the water-sealed flame-retardant tank (12) is connected with the oil tank (11).
According to the embodiment of the invention, the kiln tail gas sealing device further comprises a tail gas water sealing tank (16), wherein the tail gas water sealing tank (16) is respectively connected with the tail gas pipeline (15) and the kiln tail sealing cover (4).
According to the embodiment of the invention, the discharge screw conveyor (5) is provided with a solid material outlet (19), and the oil tank (11) is connected with an oil conveying pump (20).
It will be understood by those skilled in the art that the features and effects described above with respect to the low temperature pyrolysis process of the residuum hydroprocessing spent catalyst are, of course, applicable to this system and will not be described in detail.
The low-temperature pyrolysis method and system for the residual oil hydrogenation spent catalyst have the beneficial effects that at least:
1. the first rotary kiln (2) and the second rotary kiln (3) can be used for deoiling the oil content of the raw materials repeatedly until the oil content is completely and completely treated, and the whole deoiling process is automated.
2. Oil gas evaporated by the first rotary kiln (2) and the second rotary kiln (3) can be cooled by an oil gas cooling system in time, so that internal temperature parameters of the first rotary kiln and the second rotary kiln can be accurately controlled.
3. Oil gas can be discharged in time, and the oil gas concentration in the first rotary kiln (2) and the second rotary kiln (3) is not too high, so that the internal pressure of the first rotary kiln and the second rotary kiln can be accurately controlled.
4. After the non-condensable oil gas returns to the first rotary kiln (2) and the second rotary kiln (3), the interior of the first rotary kiln and the second rotary kiln is kept in a micro-negative pressure state, so that the sealing and pressure bearing are reduced, and the safety of production is effectively ensured.
5. The feeding equipment, the discharging equipment, the liquid oil recovery equipment and the oil gas self-circulation equipment are all designed in a structure integration way, and the feeding equipment, the discharging equipment, the liquid oil recovery equipment and the oil gas self-circulation equipment are all connected together, so that the structure integration of the whole system is realized, further, all processes of feeding, discharging, liquid oil recovery, oil gas self-circulation and the like are automatically, continuously and industrially operated, the whole process does not need to change operating places, unnecessary heat loss can be effectively prevented, and the electric energy consumption is favorably reduced.
6. The invention does not discharge any harmful tail gas, thereby being beneficial to environmental protection.
7. The invention can recover a large amount of liquid oil, and the recovered liquid oil can be applied to a plurality of aspects, such as selling as fuel oil, thereby creating great economic value and the like.
8. The whole treatment process does not need to add any treatment reagent from beginning to end, not only can save a large amount of funds, but also thoroughly avoids the generation of new impurities, achieves multiple purposes and obtains good comprehensive benefits.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic process flow diagram of a process for the low temperature pyrolysis of a residuum hydroprocessing spent catalyst in accordance with one embodiment of the present invention;
fig. 2 is a schematic view of the structure of a low-temperature pyrolysis system of a residuum-hydrogenating spent catalyst in one embodiment according to the present invention.
Reference numerals:
1-feeding screw conveyor, 2-first rotary kiln, 3-second rotary kiln, 4-kiln tail sealing cover, 5-discharging screw conveyor, 6-cooling water inlet pipe, 7-cooling water outlet pipe, 8-receiving barrel, 9-surface cooling pipeline, 10-oil-water separator, 11-oil tank, 12-water sealing flame retardant tank, 13-water ring vacuum pump, 14-circulating water tank, 15-tail gas pipeline, 16-tail gas water sealing tank, 17-kiln head sealing cover, 18-oil-gas pipeline, 19-solid material outlet, 20-oil transfer pump and 21-heat exchanger.
Detailed Description
The invention is described in further detail below with reference to specific embodiments and with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. In addition, the examples are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present specification, the terms "connect", "mount", "fix", and the like are to be understood in a broad sense, for example, "connect" may be a fixed connection, a detachable connection, or an integral connection; can be directly connected or indirectly connected through an intermediate medium; mechanical connection, circuit connection, and the like are possible. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the description of the present specification, "a plurality" means two or more unless specifically limited otherwise. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In the description of the present specification, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation. The use of the phrase "comprising one of the elements does not exclude the presence of other like elements in the process, method, article, or apparatus that comprises the element.
In the description of the present specification, it is to be noted that unless otherwise explicitly specified or limited, the terms "forward direction, reverse direction, first, second, left, right, and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance, unique positional relationships, quantitative limitations, absolute procedures, or implicitly indicating the number of technical features indicated, and the specific meaning of the terms in the present specification may be understood according to specific circumstances by those of ordinary skill in the art.
Technical principle of the invention
The inventor of the present invention has found in research that, in the prior art, there is no particularly effective treatment method for the residual oil hydrogenation spent catalyst, the prior treatment method is generally a simple heating treatment, the treatment equipment is generally a heating reaction kettle, and the prior treatment technology for the residual oil hydrogenation spent catalyst has at least the following technical defects:
(1) during heating treatment, oil is gasified, so that the pressure in the reaction kettle is quickly increased, the reaction is slowed down and even stopped, and the sealing performance of the reaction kettle is reduced;
(2) during heating treatment, oil is gasified, so that the concentration of oil and gas in a reaction kettle is increased suddenly, the gasification temperature is increased, the volatilization efficiency of the oil and gas is slowed, more heat energy (electric heating) is needed for oil gasification, and the production cost is greatly increased;
(3) during heating treatment, the oil content gasification condition is unstable, so that the technological parameters such as temperature, pressure and the like in a reaction kettle cannot be accurately controlled, the oil content cannot be completely and thoroughly treated, and continuous production cannot be realized;
(4) during heating treatment, discharged oil gas cannot be cooled in time, a large amount of liquid oil contained in the oil gas cannot be effectively recovered, the oil gas is directly discharged to pollute the environment, and a large amount of capital investment is required during oil gas purification treatment;
(5) during the heating process, can only intermittent type formula heating process, a batch material has been handled and has been cooled down, discharges and carries out next batch to need the cooperation of a plurality of reation kettle to use, the frequent switching operation place of raw materials not only wastes time and energy, has occupied a large amount of operating space, but also leads to the production incident easily.
(6) During heating treatment, temperature rise and temperature reduction are required frequently, energy consumption is high, treatment capacity is low, a large amount of manpower and material resources are wasted, and automatic, large-batch and industrial operation is difficult to perform.
Based on the above research, the inventor of the present invention has found that, on the basis of a lot of creative work, the inventor designs a unique technical scheme of the present invention, and mainly has the following 8 important technical improvements, thereby successfully solving the above-mentioned defects of the prior art:
1. automatic raw material conveying:
according to the embodiment of the invention, as shown in fig. 1 and 2, the feeding screw conveyor (1) is used for conveying raw materials to sequentially pass through the first rotary kiln (2) and the second rotary kiln (3) for deoiling, and the whole conveying process realizes automatic operation.
2. Automatic material collection:
according to the embodiment of the invention, as shown in fig. 1 and fig. 2, the deoiled solid material leaves the feeding screw conveyor (1) and enters the kiln tail sealing cover (4), then falls from the kiln tail sealing cover (4) and enters the discharging screw conveyor (5), the cooling water inlet pipe (6) and the cooling water outlet pipe (7) are communicated with cold water, the solid material falls into the receiving barrel (8) after being cooled, and the whole material collecting process realizes automatic operation.
3. Multiple oil gasification treatment:
according to the embodiment of the invention, as shown in fig. 1 and fig. 2, a plurality of first rotary kilns (2) and a plurality of second rotary kilns (3) can be arranged, so that the first rotary kiln (2) and the second rotary kilns (3) can be used for repeatedly deoiling the oil content of the raw materials for a plurality of times until the oil content is completely and completely processed, and the whole deoiling process is automated.
4. Recovering liquid oil:
according to the embodiment of the invention, as shown in fig. 1 and 2, primary oil gas and secondary oil gas generated during deoiling of the first rotary kiln (2) and the second rotary kiln (3) are sequentially cooled through the surface cooling pipeline (9), liquid oil is separated through the oil-water separator (10), the liquid oil enters the oil tank (11), so that a large amount of liquid oil contained in the oil gas is recovered, and the whole liquid oil recovery process realizes automatic operation.
5. Oil gas self-circulation:
according to the embodiment of the invention, as shown in fig. 1 and fig. 2, primary oil gas and secondary oil gas sequentially pass through a surface cooling pipeline (9), an oil-water separator (10) and a heat exchanger (21) to form liquid oil and non-condensable gas, the liquid oil enters an oil tank (11) to be recovered, the non-condensable gas sequentially passes through a water-seal flame-retardant tank (12), a water ring vacuum pump (13), a circulating water tank (14), a tail gas pipeline (15) and a tail gas water-seal tank (16) and then enters a kiln tail sealing cover (4) and a kiln head sealing cover (17), oil gas in a furnace is blown out of a hearth to form an oil gas self-circulation passage, and the unique design of the oil gas self-circulation passage has at least three advantages:
oil gas evaporated by the first rotary kiln (2) and the second rotary kiln (3) can be cooled by an oil gas cooling system in time, so that internal temperature parameters of the first rotary kiln and the second rotary kiln can be accurately controlled;
oil gas can be discharged in time, so that the oil gas concentration in the first rotary kiln (2) and the second rotary kiln (3) is not too high, and the internal pressure of the first rotary kiln and the second rotary kiln can be accurately controlled;
thirdly, after the non-condensable oil gas returns to the first rotary kiln (2) and the second rotary kiln (3), the interior of the first rotary kiln and the second rotary kiln is kept in a micro negative pressure state, so that the sealing and pressure bearing are reduced, and the safety of production is ensured powerfully.
As mentioned above, the process parameters such as temperature, pressure and the like of the first rotary kiln (2) and the second rotary kiln (3) can be accurately controlled, so that the oil content can be completely and thoroughly treated, and the continuous and high-efficiency production can be realized. In addition, the whole oil-gas self-circulation process also realizes automatic operation.
6. The integrated structure design:
through a great deal of creative research, the inventor of the invention carries out the integrated structure design of the system of the low-temperature pyrolysis method of the residual oil hydrogenation waste catalyst, which is described in the following points:
(1) structural integration of feeding equipment
According to the embodiment of the invention, as shown in fig. 2, the feeding screw conveyor (1) penetrates through the first rotary kiln (2) and the second rotary kiln (3), so that the feeding screw conveyor (1) can convey raw materials to sequentially pass through the first rotary kiln (2) and the second rotary kiln (3) for deoiling respectively, and the whole deoiling process realizes automatic operation.
(2) Structure integration of discharging equipment
According to the embodiment of the invention, as shown in fig. 2, the discharging screw conveyor (5) is connected with the kiln tail sealing cover (4), the cooling water inlet pipe (6) and the cooling water outlet pipe (7) are both connected with the discharging screw conveyor (5), and the receiving barrel (8) is arranged below the discharging screw conveyor (5).
(3) Structure integration of liquid oil recovery equipment
According to the embodiment of the invention, as shown in fig. 2, the surface cooling pipeline (9), the oil-water separator (10), the oil tank (11) and other equipment used for liquid oil recovery are connected together in a uniform body, and the whole liquid oil recovery process realizes automatic operation.
(4) Structure integration of oil gas self-loopa equipment
According to the embodiment of the invention, as shown in fig. 2, the surface cooling pipeline (9), the oil-water separator (10), the oil tank (11), the water-sealed flame-retardant tank (12), the water-ring vacuum pump (13), the circulating water tank (14), the tail gas pipeline (15) and other equipment used for oil-gas self-circulation are connected together in a uniform body, and the whole oil-gas self-circulation process realizes automatic operation.
(5) Structural integration of the entire system
As above, feeding equipment, discharging equipment, liquid oil recovery equipment, four of oil gas self-loopa equipment are the structure integration design, and feeding equipment, discharging equipment, liquid oil recovery equipment, four of oil gas self-loopa equipment all link together, thereby the structure integration of entire system has been realized, and then make all processes such as feeding, the ejection of compact, liquid oil recovery, oil gas self-loopa all realize automation, serialization, industrial operation, whole process need not to alternate the workplace, can effectively prevent unnecessary calorific loss, be favorable to reducing the electric energy quantity.
7. The recovered product creates economic value:
the invention can recover a large amount of liquid oil, and the recovered liquid oil can be applied to a plurality of aspects, such as selling as fuel oil, thereby creating great economic value and the like.
8. Without any treatment reagents:
it should be noted that, the present invention also has a largest technical achievement: the whole treatment process does not need to add any treatment reagent from beginning to end, not only can save a large amount of funds, but also thoroughly avoids the generation of new impurities, achieves multiple purposes and obtains good comprehensive benefits.
Detailed description of the invention
The invention will be further described with reference to the following specific examples, which are provided for illustrative purposes only and are not to be construed as limiting the invention in any way, in conjunction with fig. 1 and 2. In addition, in the following examples, if not specifically mentioned, all the equipment and materials used are commercially available.
EXAMPLE 1
First, experiment raw materials
1. Raw materials:
the residual oil hydrogenation waste catalyst is from a certain oil refinery, and comprises the following components in percentage by weight: 65% of alumina, 4% of molybdenum, 15% of vanadium pentoxide and 15% of oil, wherein the residual oil hydrogenation waste catalyst has the physical and chemical characteristics that: diesel odor, black clover shaped solid.
2. Equipment:
feeding screw conveyer (1), first rotary kiln (2), second rotary kiln (3), kiln tail sealed cowling (4), ejection of compact screw conveyer (5), cooling water inlet tube (6), cooling water outlet pipe (7), connect storage bucket (8), table cold pipeline (9), oil water separator (10), oil tank (11), water seal fire-retardant jar (12), water ring vacuum pump (13), circulating water tank (14), tail gas pipeline (15), tail gas water seal jar (16), kiln head sealed cowling (17), oil gas pipeline (18), oil transfer pump (20) and heat exchanger (21), wherein, first rotary kiln (2) and second rotary kiln (3) are sealed external heating rotary furnace.
II, an experiment step:
s100, deoiling raw materials: the method comprises the following steps of (1) utilizing a feeding screw conveyor (1) to sequentially pass through a first rotary kiln (2) and a second rotary kiln (3) to respectively carry out deoiling, wherein the feeding screw conveyor (1) rotates at 2 Hz, the first rotary kiln (2) and the second rotary kiln (3) rotate at 20 Hz, and the deoiling time of the raw materials in the first rotary kiln (2) and the second rotary kiln (3) is 3 hours;
s200, primary oil gasification: the temperature in the first rotary kiln (2) is 350 ℃, the negative pressure in the kiln is 0.005MPa, and oil is gasified to form primary oil gas;
s300, secondary oil gasification: the temperature in the second rotary kiln (3) is 600 ℃, the negative pressure in the kiln is 0.008MPa, and secondary oil gas is formed after oil is gasified;
s400, collecting materials: the solid materials after deoiling leave the feeding screw conveyor (1) and enter the kiln tail sealing cover (4), then fall from the kiln tail sealing cover (4) and enter the discharging screw conveyor (5), the discharging screw conveyor (5) rotates at 3 Hz, a cooling water inlet pipe (6) and a cooling water outlet pipe (7) are communicated with cold water, and the solid materials fall into a material receiving barrel (8) after being cooled;
s500, liquid oil recovery: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9) and an oil-water separator (10), are cooled into liquid oil and then enter an oil tank (11), and an oil transfer pump (20) is started to recover the liquid oil;
s600, oil gas self-circulation: primary oil gas and secondary oil gas loop through table cold pipe way (9), oil water separator (10) and heat exchanger (21), form liquid oil and noncondensable gas, liquid oil gets into oil tank (11) and retrieves, noncondensable gas loops through water seal fire-retardant jar (12), water ring vacuum pump (13), circulating water tank (14), tail gas pipeline (15), it is interior to go into kiln tail sealed cowling (4) and kiln head sealed cowling (17) behind tail gas water-sealed jar (16), use as nitrogen gas, blow off furnace with the oil gas in the stove.
Thirdly, experimental results:
(1) the solid material product was black with a slight diesel odor, indicating that most of the oil was disposed of cleanly.
(2) Liquid oil is recovered which can be used in a number of applications, for example, to create economic value again when fuel oil is sold.
(3) No harmful tail gas is discharged, which is beneficial to environmental protection.
(4) The whole treatment process does not need to add any treatment reagent from beginning to end, not only can save a large amount of funds, but also thoroughly avoids the generation of new impurities, achieves multiple purposes and obtains good comprehensive benefits
(5) The whole processes of feeding, discharging, liquid oil recovery, oil gas self-circulation and the like all realize automatic operation, a large amount of manpower and material resources are saved, the whole process does not need to change operation places, unnecessary heat loss can be effectively prevented, and the reduction of the electric energy consumption is facilitated.
EXAMPLE 2
First, experiment raw materials
1. Raw materials:
the residual oil hydrogenation waste catalyst is from a certain oil refinery, and comprises the following components in percentage by weight: 65% of alumina, 4% of molybdenum, 15% of vanadium pentoxide and 15% of oil, wherein the residual oil hydrogenation waste catalyst has the physical and chemical characteristics that: diesel odor, black clover shaped solid.
2. Equipment:
feeding screw conveyer (1), first rotary kiln (2), second rotary kiln (3), kiln tail sealed cowling (4), ejection of compact screw conveyer (5), cooling water inlet tube (6), cooling water outlet pipe (7), connect storage bucket (8), table cold pipeline (9), oil water separator (10), oil tank (11), water seal fire-retardant jar (12), water ring vacuum pump (13), circulating water tank (14), tail gas pipeline (15), tail gas water seal jar (16), kiln head sealed cowling (17), oil gas pipeline (18), oil transfer pump (20) and heat exchanger (21), wherein, first rotary kiln (2) and second rotary kiln (3) are sealed external heating rotary furnace.
II, an experiment step:
s100, deoiling raw materials: the method comprises the following steps of (1) utilizing a feeding screw conveyor (1) to sequentially pass through a first rotary kiln (2) and a second rotary kiln (3) for deoiling respectively, wherein the feeding screw conveyor (1) rotates at 5 Hz, the first rotary kiln (2) and the second rotary kiln (3) rotate at 20 Hz, and the deoiling time of the raw materials in the first rotary kiln (2) and the second rotary kiln (3) is 3 hours;
s200, primary oil gasification: the temperature in the first rotary kiln (2) is 500 ℃, the negative pressure in the kiln is 0.005MPa, and oil is gasified to form primary oil gas;
s300, secondary oil gasification: the temperature in the second rotary kiln (3) is 600 ℃, the negative pressure in the kiln is 0.008MPa, and secondary oil gas is formed after oil is gasified;
s400, collecting materials: the solid materials after deoiling leave the feeding screw conveyor (1) and enter the kiln tail sealing cover (4), then fall from the kiln tail sealing cover (4) and enter the discharging screw conveyor (5), the discharging screw conveyor (5) rotates at 10 Hz, a cooling water inlet pipe (6) and a cooling water outlet pipe (7) are communicated with cold water, and the solid materials fall into a material receiving barrel (8) after being cooled;
s500, liquid oil recovery: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9) and an oil-water separator (10), are cooled into liquid oil and then enter an oil tank (11), and an oil transfer pump (20) is started to recover the liquid oil;
s600, oil gas self-circulation: primary oil gas and secondary oil gas loop through table cold pipe way (9), oil water separator (10) and heat exchanger (21), form liquid oil and noncondensable gas, liquid oil gets into oil tank (11) and retrieves, noncondensable gas loops through water seal fire-retardant jar (12), water ring vacuum pump (13), circulating water tank (14), tail gas pipeline (15), it is interior to go into kiln tail sealed cowling (4) and kiln head sealed cowling (17) behind tail gas water-sealed jar (16), use as nitrogen gas, blow off furnace with the oil gas in the stove.
Thirdly, experimental results:
(1) the solid material product is black, the smell of the diesel oil basically disappears, and most of oil content is completely treated.
(2) Liquid oil is recovered which can be used in a number of applications, for example, to create economic value again when fuel oil is sold.
(3) No harmful tail gas is discharged, which is beneficial to environmental protection.
(4) The whole treatment process does not need to add any treatment reagent from beginning to end, not only can save a large amount of funds, but also thoroughly avoids the generation of new impurities, achieves multiple purposes and obtains good comprehensive benefits.
(5) The whole processes of feeding, discharging, liquid oil recovery, oil gas self-circulation and the like all realize automatic operation, a large amount of manpower and material resources are saved, the whole process does not need to change operation places, unnecessary heat loss can be effectively prevented, and the reduction of the electric energy consumption is facilitated.
EXAMPLE 3
First, experiment raw materials
1. Raw materials:
the residual oil hydrogenation waste catalyst is from a certain oil refinery, and comprises the following components in percentage by weight: 65% of alumina, 4% of molybdenum, 15% of vanadium pentoxide and 15% of oil, wherein the residual oil hydrogenation waste catalyst has the physical and chemical characteristics that: diesel odor, black clover shaped solid.
2. Equipment:
feeding screw conveyer (1), first rotary kiln (2), second rotary kiln (3), kiln tail sealed cowling (4), ejection of compact screw conveyer (5), cooling water inlet tube (6), cooling water outlet pipe (7), connect storage bucket (8), table cold pipeline (9), oil water separator (10), oil tank (11), water seal fire-retardant jar (12), water ring vacuum pump (13), circulating water tank (14), tail gas pipeline (15), tail gas water seal jar (16), kiln head sealed cowling (17), oil gas pipeline (18), oil transfer pump (20) and heat exchanger (21), wherein, first rotary kiln (2) and second rotary kiln (3) are sealed external heating rotary furnace.
II, an experiment step:
s100, deoiling raw materials: the method comprises the following steps of (1) utilizing a feeding screw conveyor (1) to sequentially pass through a first rotary kiln (2) and a second rotary kiln (3) to respectively carry out deoiling, wherein the feeding screw conveyor (1) rotates at 3 Hz, the first rotary kiln (2) and the second rotary kiln (3) rotate at 20 Hz, and the deoiling time of the raw materials in the first rotary kiln (2) and the second rotary kiln (3) is 3 hours;
s200, primary oil gasification: the temperature in the first rotary kiln (2) is 300 ℃, the negative pressure in the kiln is 0.005MPa, and oil is gasified to form primary oil gas;
s300, secondary oil gasification: the temperature in the second rotary kiln (3) is 400 ℃, the negative pressure in the kiln is 0.008MPa, and oil is gasified to form secondary oil gas;
s400, collecting materials: the solid materials after deoiling leave the feeding screw conveyor (1) and enter the kiln tail sealing cover (4), then fall from the kiln tail sealing cover (4) and enter the discharging screw conveyor (5), the discharging screw conveyor (5) rotates at 7 Hz, a cooling water inlet pipe (6) and a cooling water outlet pipe (7) are communicated with cold water, and the solid materials fall into a material receiving barrel (8) after being cooled;
s500, liquid oil recovery: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9) and an oil-water separator (10), are cooled into liquid oil and then enter an oil tank (11), and an oil transfer pump (20) is started to recover the liquid oil;
s600, oil gas self-circulation: primary oil gas and secondary oil gas loop through table cold pipe way (9), oil water separator (10) and heat exchanger (21), form liquid oil and noncondensable gas, liquid oil gets into oil tank (11) and retrieves, noncondensable gas loops through water seal fire-retardant jar (12), water ring vacuum pump (13), circulating water tank (14), tail gas pipeline (15), it is interior to go into kiln tail sealed cowling (4) and kiln head sealed cowling (17) behind tail gas water-sealed jar (16), use as nitrogen gas, blow off furnace with the oil gas in the stove.
Thirdly, experimental results:
(1) the solid material product is black, the smell of the diesel oil basically disappears, and most of oil content is completely treated.
(2) Liquid oil is recovered which can be used in a number of applications, for example, to create economic value again when fuel oil is sold.
(3) No harmful tail gas is discharged, which is beneficial to environmental protection.
(4) The whole treatment process does not need to add any treatment reagent from beginning to end, not only can save a large amount of funds, but also thoroughly avoids the generation of new impurities, achieves multiple purposes and obtains good comprehensive benefits.
(5) The whole processes of feeding, discharging, liquid oil recovery, oil gas self-circulation and the like all realize automatic operation, a large amount of manpower and material resources are saved, the whole process does not need to change operation places, unnecessary heat loss can be effectively prevented, and the reduction of the electric energy consumption is facilitated.
It should be specifically noted that technical features and advantages which are known in the prior art or already described are easily understood by those skilled in the art and are not described in detail herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and the present invention may be variously modified and changed. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A low-temperature pyrolysis method of residual oil hydrogenation spent catalyst is characterized by comprising the following steps:
s100, deoiling raw materials: the raw materials are sequentially subjected to deoiling through a first rotary kiln (2) and a second rotary kiln (3) by using a feeding screw conveyor (1);
s200, primary oil gasification: the temperature in the first rotary kiln (2) is 300-;
s300, secondary oil gasification: the temperature in the second rotary kiln (3) is 300-;
s400, collecting materials: the solid materials after deoiling leave the feeding screw conveyor (1) and enter a kiln tail sealing cover (4), then fall from the kiln tail sealing cover (4) and enter a discharging screw conveyor (5), a cooling water inlet pipe (6) and a cooling water outlet pipe (7) are communicated with cold water, and the solid materials fall into a material receiving barrel (8) after being cooled;
s500, liquid oil recovery: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9) and an oil-water separator (10), are cooled into liquid oil and then enter an oil tank (11) for recovery;
s600, oil gas self-circulation: the primary oil gas and the secondary oil gas sequentially pass through a surface cooling pipeline (9), an oil-water separator (10) and a heat exchanger (21) to form liquid oil and non-condensable gas, the liquid oil enters an oil tank (11) to be recovered, the non-condensable gas sequentially passes through a water seal flame-retardant tank (12), a water ring vacuum pump (13), a circulating water tank (14), a tail gas pipeline (15) and a tail gas water seal tank (16) and then enters a kiln tail sealing cover (4) and a kiln head sealing cover (17), and the oil gas in the furnace is blown out of a hearth to form an oil gas self-circulation passage.
2. The method for the low temperature pyrolysis of residual oil hydrogenation spent catalyst according to claim 1, wherein the non-condensable gas forms liquid oil when passing through the water-sealed fire-retardant tank (12) in step S600, and the liquid oil is recycled through the oil tank (11).
3. A process for the low temperature pyrolysis of a spent residue hydrogenation catalyst according to claim 1, wherein the first rotary kiln (2) and the second rotary kiln (3) are sealed external heating rotary furnaces.
4. A process for the low temperature pyrolysis of a residuum hydrogenating dead catalyst according to claim 1, characterized in that the first rotary kiln (2) and the second rotary kiln (3) are rotated at 20 hz.
5. The low temperature pyrolysis method of residuum spent hydroprocessing catalyst according to claim 1, characterized in that the feed auger (1) rotates at 2-5 hz and the discharge auger (5) rotates at 3-10 hz.
6. A process for the low temperature pyrolysis of a residuum hydrogenating dead catalyst according to claim 1, characterized in that the time for the deoiling of the feedstock in the first rotary kiln (2) and the second rotary kiln (3) is 3 hours.
7. A system suitable for use in a low temperature pyrolysis process of a residuum hydroprocessing spent catalyst as described in any one of claims 1-6, the system comprising: the device comprises a feeding spiral conveyor (1), a first rotary kiln (2), a second rotary kiln (3), a kiln tail sealing cover (4), a discharging spiral conveyor (5), a cooling water inlet pipe (6), a cooling water outlet pipe (7), a receiving barrel (8), a surface cooling pipeline (9), an oil-water separator (10), an oil tank (11), a water-seal flame-retardant tank (12), a water ring vacuum pump (13), a circulating water tank (14), a tail gas pipeline (15), a kiln head sealing cover (17), an oil-gas pipeline (18) and a heat exchanger (21);
the feeding screw conveyor (1) penetrates through the first rotary kiln (2) and the second rotary kiln (3) so as to convey raw materials to sequentially pass through the first rotary kiln (2) and the second rotary kiln (3) for deoiling respectively;
the first rotary kiln (2) is connected with the kiln head sealing cover (17), the second rotary kiln (3) is connected with the kiln tail sealing cover (4), the kiln head sealing cover (17) and the kiln tail sealing cover (4) are both connected with the oil-gas pipeline (18), the surface cooling pipeline (9) is connected with the oil-gas pipeline (18), the oil-water separator (10) is connected with the surface cooling pipeline (9), and the oil tank (11) is connected with the oil-water separator (10);
the heat exchanger (21) is respectively connected with the oil-water separator (10) and the oil tank (11), the water-sealed flame-retardant tank (12) is connected with the heat exchanger (21), the water-ring vacuum pump (13) is connected with the water-sealed flame-retardant tank (12), the circulating water tank (14) is connected with the water-ring vacuum pump (13), the tail gas pipeline (15) is connected with the circulating water tank (14), and the kiln head sealing cover (17) and the kiln tail sealing cover (4) are both connected with the tail gas pipeline (15);
the discharging screw conveyor (5) is connected with the kiln tail sealing cover (4), the cooling water inlet pipe (6) and the cooling water outlet pipe (7) are both connected with the discharging screw conveyor (5), and the receiving barrel (8) is arranged below the discharging screw conveyor (5).
8. A low temperature pyrolysis system of residuum hydrogenation spent catalyst according to claim 7, characterized in that the water-sealed flame retardant tank (12) is connected with the oil tank (11).
9. The system for the low-temperature pyrolysis of a residuum hydrogenation spent catalyst according to claim 7, further comprising a tail gas water seal tank (16), wherein the tail gas water seal tank (16) is connected with the tail gas pipeline (15) and the kiln tail seal cover (4), respectively.
10. The low temperature pyrolysis system of residuum spent hydrogenation catalyst according to claim 7, characterized in that the discharge screw conveyor (5) is provided with a solid outlet (19), and the oil tank (11) is connected with an oil transfer pump (20).
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| US6005149A (en) * | 1998-08-18 | 1999-12-21 | Engineering, Separation & Recycling, Ltd. Co. | Method and apparatus for processing organic materials to produce chemical gases and carbon char |
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