CN114672631A - Method for regulating and controlling full-thickness structure-stress-performance uniformity of ultra-thick forging of large hydrogenation reactor - Google Patents

Method for regulating and controlling full-thickness structure-stress-performance uniformity of ultra-thick forging of large hydrogenation reactor Download PDF

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CN114672631A
CN114672631A CN202210305337.8A CN202210305337A CN114672631A CN 114672631 A CN114672631 A CN 114672631A CN 202210305337 A CN202210305337 A CN 202210305337A CN 114672631 A CN114672631 A CN 114672631A
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CN114672631B (en
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蒋文春
谷文斌
王金光
李志杰
杨靖
张凯
王迎君
涂善东
袁继军
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Sinopec Engineering Inc
China University of Petroleum East China
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/005Modifying the physical properties by deformation combined with, or followed by, heat treatment of ferrous alloys
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18Hardening; Quenching with or without subsequent tempering
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • C21D1/30Stress-relieving
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D3/00Diffusion processes for extraction of non-metals; Furnaces therefor
    • C21D3/02Extraction of non-metals
    • C21D3/06Extraction of hydrogen
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/002Bainite

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Abstract

The invention discloses a method for regulating and controlling the full-thickness structure-stress-performance uniformity of an ultra-thick forging of a large hydrogenation reactor, which mainly comprises the following steps: after forging, cooling the forging to 700 +/-10 ℃ at a cooling speed of 20-30 ℃/h, and preserving heat for 15-20 h; heating to 1040-1080 ℃ in a gradual heating mode, and keeping for a certain time; cooling to 660-720 ℃ in a gradual cooling mode, keeping for a certain time, then cooling to 350-400 ℃, and naturally cooling to room temperature for rough machining; after rough machining is finished, heating to 920-950 ℃, keeping for a certain time, then quickly quenching, and cooling to 200-250 ℃ after quenching; transferring the quenched product to a heat treatment furnace, heating to 660-720 ℃ in a gradual heating mode, and keeping for a certain time; then cooling to below 300 ℃ at a cooling speed of 20-30 ℃/h, and then discharging and air cooling; according to the invention, the post-forging heat treatment process and the heat treatment process are combined, so that the limitation that the core structure and the stress cannot be regulated and controlled in the traditional process is broken, and the synchronous regulation and control of the structure, the performance and the stress in the full thickness direction are realized.

Description

Method for regulating and controlling full-thickness structure-stress-performance uniformity of ultra-thick forging of large hydrogenation reactor
Technical Field
The invention relates to the technical field of hydrogenation reactor preparation, in particular to a full-thickness structure-stress-performance uniformity regulation and control method for an ultra-thick forging of a large hydrogenation reactor.
Background
The hydrogenation reactor is the core equipment of a petrochemical hydrogenation device, is the most important container in petrochemical production, has harsh working conditions, and can work in a high-temperature and high-pressure environment, and the contact medium is corrosive media such as oil gas, hydrogen sulfide and the like, so that the requirement on service safety of the hydrogenation reactor is extremely high. With the development of million tons of oil refining and million tons of ethylene, the hydrogenation reactor develops towards the direction of super-wall thickness and super-diameter, so that the wall thickness of the hydrogenation reactor is over-thick, plate welding cannot be carried out, only hot forging manufacture can be adopted (the recrystallization temperature is higher, and the cold deformation strengthening and recrystallization processes exist at the same time), the structure damage is serious in the hot forging process, the crystal grains are thick, meanwhile, the forging plastic deformation of the super-thick cylinder is severe, large thermal stress is generated, the super-thick cylinder is easy to crack in subsequent use, and the forge piece needs to be subjected to heat treatment to improve the structure and the performance of the forge piece. At present, the heat treatment method commonly used in engineering includes a plurality of heat treatment processes such as normalizing, tempering, rough machining and then normalizing, tempering and the like, for example, the heat treatment process disclosed in chinese patent CN 105385814A. However, the prior heat treatment method is difficult to realize the synchronous recovery of the full-wall thickness structure performance, and the residual stress is large, so that the uniformity of the performance along the wall thickness direction is poor. Therefore, the tissue-stress-performance synchronous regulation and control of the full thickness of the ultra-thick forging of the large hydrogenation reactor are needed to ensure the intrinsic safety of the hydrogenation reactor. In order to solve the problems, the invention provides a full-thickness structure-stress-performance regulation and control method for an ultra-thick forging of a large hydrogenation reactor, which breaks through the limitation that the core structure and stress cannot be regulated and controlled in the traditional process, and realizes synchronous regulation and control of the structure, the performance and the stress in the full-thickness direction.
Disclosure of Invention
The invention aims to provide a full-thickness structure-stress-performance uniformity regulation and control method for an ultra-thick forging of a large hydrogenation reactor, which breaks through the limitation that the core structure and stress cannot be regulated and controlled by the traditional process, and realizes synchronous regulation and control of the structure, the performance and the stress in the full-thickness direction.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a full-thickness structure-stress-performance uniformity regulation and control method for an ultra-thick forging of a large hydrogenation reactor, which comprises the following steps:
(1) rapidly heating the steel ingot to 300-350 ℃, then heating to 650-700 ℃ at a heating rate not more than 56 ℃/h, and preserving heat for 4-6 h; then, heating the steel ingot to 1180 +/-10 ℃ in sections, and preserving heat for 2-4 hours;
the steps aim to ensure the temperature uniformity in the forging process, reduce the crystal grain damage and reduce the structure-stress-performance unevenness caused by the temperature unevenness;
(2) forging and forming the steel ingot within the steel ingot forging temperature range in the step (1), and controlling the forging final temperature to be not less than 850 ℃;
(3) after the forging in the step (2) is completed, transferring the forged piece into a heat treatment furnace for slow cooling, wherein the furnace entering temperature of the forged piece is above 850 ℃, then cooling to 700 +/-10 ℃ at a cooling speed of 20-30 ℃/h, and preserving heat for 15-20 h;
in the step (3), the cooling speed is controlled to be 20-30 ℃/h, so that the thermal stress generated in the cooling process can be reduced; and then, heat preservation treatment is carried out at about 700 ℃, so that the structure of the forged piece can be improved, crystal grains can be refined, the grain size can reach 6 grades or above, meanwhile, the residual stress in the forging forming process is partially eliminated, the hardness is reduced, and the residual stress can be reduced to 200-260 MPa.
(4) On the basis of the step (3), heating to 1040-1080 ℃ in a gradual heating manner, and keeping for a certain time t1
The step (4) is used for further refining the crystal grains of the forge piece;
(5) cooling to 660-720 ℃ in a gradual cooling way and keeping for a certain time t2(ii) a Then gradually cooling to 350-400 ℃, and then naturally cooling to room temperature for rough machining;
the step (5) has the effects of realizing the dehydrogenation treatment of the forge piece, reducing the residual stress and recovering the toughness and the plasticity of the forge piece;
(6) after rough machining is finished, quickly heating to 400 ℃, then heating to 920-950 ℃ in a gradual heating mode, and keeping for a certain time t3(ii) a Then transferring the forged piece to a quenching bath, quenching the forged piece at a cooling speed of not less than 5 ℃/h, and cooling to 200-250 ℃ after quenching;
the steps are quenching treatment, in order to ensure the quenching cooling speed, the water circulation amount of a quenching tank needs to be increased, the forge piece is placed in the quenching tank with a rotary platform at the bottom, the forge piece is rotated by a propeller, the rapid cooling of the forge piece is realized by adopting a rotary water injection mode, a surface gasification film of the forge piece in the quenching process can be broken by adopting the rotary water injection mode, the cooling speed of the forge piece is ensured to reach more than 5 ℃/min, the forge piece is finally ensured to form a lower bainite tissue along the full thickness direction, and the forge piece tissue is improved;
(7) transferring the quenched forge piece to a heat treatment furnace, slowly cooling to 150 +/-10 ℃, and keeping for 3-6 hours; then gradually heating to 660-720 ℃, and keeping for a certain time t4(ii) a Finally, cooling to below 300 ℃ at a cooling speed of 20-30 ℃/h, and discharging and air cooling;
the step (7) is used for further eliminating the residual stress of the forging, reducing the residual stress to be below 100MPa and recovering the toughness and the plasticity of the forging;
in the above stepsIn steps (4) to (7), the t1=(0.01δ+4)h,t2=(0.04δ+2)h,t3=(0.02δ+3)h,t4δ is the forging wall thickness in mm (0.02 δ +10) h.
Further, the segmented temperature rising mode in the step (1) is as follows: heating the steel ingot to 800 +/-20 ℃ at a heating rate of less than 45 ℃/h, and preserving heat for 1-2 h; after the temperature is stable, heating the steel ingot to 900 +/-20 ℃ at the same heating rate, and preserving the heat for 1-2 hours; then, heating to 1000 +/-20 ℃ at the same heating rate, and preserving heat for 1-2 h; and finally, heating to 1180 +/-10 ℃ at the same heating speed, and preserving heat for 2-4 hours.
According to the technical scheme, the temperature of the steel ingot is gradually increased before forging, so that the temperature difference between the core part and the surface of the steel ingot can be reduced, and the uniformity of the structure, the stress and the performance of a forging piece in the full thickness direction can be guaranteed in the forging process.
Further, in the step (2), the temperature of the forged piece is controlled to be not less than 850 ℃ in the forging process, if the temperature is lower than 850 ℃, the forged piece needs to be returned to the furnace to be heated to 1180 +/-10 ℃, and heat is preserved for 1-2 hours.
In the technical scheme, the temperature of the forge piece is controlled to be not less than 850 ℃, so that the forging forming is facilitated, and the tissue damage in the hot forging process is reduced; when the temperature is lower than 850 ℃, the furnace needs to be returned to 1180 +/-10 ℃, the temperature is kept for 1-2 hours, the residual stress generated by deformation and forging in the forging process can be reduced, and then the forging process is repeated.
Further, the gradual temperature rise manner in the steps (4), (6), and (7) is: gradually heating the forging piece at a heating rate of not more than 35 ℃/h for n times to raise the temperature to a planned heating target temperature, wherein the temperature is raised by delta T each timeiKeeping the temperature at a certain value for a certain time t after each temperature risei
Wherein, Δ TiDetermining according to the wall thickness delta of the forged piece: when delta<At 200mm,. DELTA.Ti130 ℃ under normal temperature; when delta is more than or equal to 200mm and less than 300mm, delta TiThe temperature is 100 ℃; when delta is more than or equal to 300mm and less than 400mm, delta Ti=80℃;
The calculation mode of the gradual temperature rise times n is as follows:
Figure BDA0003564805560000031
n is an integer; wherein T is a planned heating target temperature, TaThe temperature of the forged piece before temperature rise;
holding time tiThe calculation formula of (2) is as follows: t is ti=(10+2ni) min, wherein niFor the ith heating, ni=i,i=1,2…,n。
In the technical scheme, the temperature rising times, the temperature rising temperature and the heat preservation time are determined according to the wall thickness of the forging piece in a gradual temperature rising mode, so that the temperature uniformity of the thick-wall forging piece along the wall thickness direction in the temperature rising process can be ensured, and the temperature difference between the core temperature and the surface temperature is not more than 5 ℃.
Further, the gradual cooling mode in the step (5) is as follows: gradually cooling the forging piece for N times at a cooling speed of less than 50 ℃/h to reduce the temperature to a preset cooling target temperature, wherein the temperature is reduced by delta T each timejAnd is kept for a certain time t after each coolingj
Wherein, Delta TjDetermining according to the wall thickness delta of the forged piece: when delta is less than 200mm, delta TjThe temperature is 200 ℃; when delta is more than or equal to 200mm and less than 300mm, delta Tj150 ℃ is set; when delta is more than or equal to 300mm and less than 400mm, delta Tj=100℃;
The calculation formula of the gradual cooling times N is as follows:
Figure BDA0003564805560000032
taking an integer from N upwards; wherein, TbThe temperature before the temperature reduction of the forge piece is carried out, and T' is the set temperature target temperature;
holding time tjThe calculation formula of (2) is as follows: t is tj=2(10+(N-2nj) Min, wherein n isjFor the j th heating, ni=i,i=1,2…,N。
In the technical scheme, the temperature reduction times, the temperature reduction temperature and the heat preservation time are determined according to the wall thickness of the forge piece in a gradual temperature reduction mode, and the temperature uniformity of the thick-wall forge piece in the wall thickness direction in the temperature reduction process can be ensured.
The beneficial effects of the invention are:
the regulating method provided by the invention aims at the ultra-thick forged piece of the large hydrogenation reactor, the synchronous regulation and control of the whole thickness structure-stress-performance of the forged piece can be realized, compared with the traditional method, the method breaks through the limitation that the traditional process can not regulate and control the core structure-stress-performance, the synchronous regulation and control of the structure, the performance and the stress of the forged piece with the thickness of 200-400 mm, even 500mm in the whole thickness direction can be realized, the forged piece can form a lower bainite structure in the whole thickness direction, the grain size can reach 8 grade, the uniformity of the structure performance is ensured, and the residual stress is reduced to be below 100 MPa; in addition, the temperature of the forging is not completely reduced after forging, but the temperature of the forging is kept at a high temperature for a period of time, so that the temperature in the full thickness direction is basically kept uniform, the structure of the forging is improved, crystal grains are refined, part of residual stress in the forging forming process is eliminated, the structure stress in the forging process is fully recovered, and the improvement of the structure, the performance and the stress of the forging by subsequent heat treatment is promoted; meanwhile, the long-time heating process after cooling is avoided, and the energy-saving and environment-friendly effects are achieved.
Drawings
FIG. 1 is a heat treatment process profile of example 1 of the present invention.
Detailed Description
The invention provides a method for regulating and controlling the whole-thickness structure-stress-performance uniformity of an ultra-thick forging of a large hydrogenation reactor, and the method is further explained in detail below in order to make the purpose, the technical scheme and the effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a full-thickness structure-stress-performance uniformity regulation and control method for an ultra-thick forging of a large hydrogenation reactor, which comprises the following steps:
(1) rapidly heating the steel ingot to 300-350 ℃, then heating to 650-700 ℃ at a heating rate of not more than 56 ℃/h, and preserving heat for 4-6 h; then heating the steel ingot to 800 +/-20 ℃ at a heating rate of less than 45 ℃/h, and preserving heat for 1-2 h; after the temperature is stable, heating the steel ingot to 900 +/-20 ℃ at the same heating rate, and preserving the heat for 1-2 hours; then, heating to 1000 +/-20 ℃ at the same heating rate, and preserving heat for 1-2 h; finally, heating to 1180 +/-10 ℃ at the same heating speed, and preserving heat for 2-4 hours;
(2) forging and forming the steel ingot within the steel ingot forging temperature range in the step (1), and controlling the forging finishing temperature to be not less than 850 ℃; controlling the temperature of the forge piece to be not less than 850 ℃ in the forging process, returning to the furnace to heat to 1180 +/-10 ℃ if the temperature is less than 850 ℃, and preserving heat for 1-2 hours;
(3) after the forging in the step (2) is completed, transferring the forged piece to a heat treatment furnace, cooling the forged piece to 700 +/-10 ℃ at a cooling speed of 20-30 ℃/h, and preserving heat for 15-20 h;
(4) on the basis of the step (3), heating to 1040-1080 ℃ in a gradual heating manner, and keeping for a certain time t1
(5) Cooling to 660-720 ℃ in a gradual cooling way and keeping for a certain time t2(ii) a Then gradually cooling to 350-400 ℃, and naturally cooling to room temperature for rough machining;
(6) quenching treatment
After rough machining is finished, quickly heating to 400 ℃, then heating to 920-950 ℃ in a gradual heating mode, and keeping for a certain time t3(ii) a Then transferring the forged piece to a quenching bath, quenching the forged piece at a cooling speed of not less than 5 ℃/h, and cooling to 200-250 ℃ after quenching;
(7) transferring the quenched forged piece to a heat treatment furnace, slowly cooling to 200 +/-10 ℃, and keeping for 3-6 h; then gradually heating to 660-720 ℃, and keeping for a certain time t4(ii) a Finally, cooling to below 300 ℃ at a cooling speed of 20-30 ℃/h, and then discharging and air cooling;
said t is1=(0.01δ+4)h,t2=(0.04δ+2)h,t3=(0.02δ+3)h,t4And d is (0.02 delta +10) h, delta is the wall thickness of the forged piece, and the unit of the wall thickness is mm.
The gradual temperature rise mode in the steps (4), (6) and (7) is as follows: gradually heating the forging piece at a heating rate of not more than 35 ℃/h for n times to raise the temperature to a planned heating target temperature, wherein the temperature is raised by delta T each timeiKeeping the temperature at a certain value for a certain time t after each temperature risei
Wherein, Delta TiDetermining according to the wall thickness delta of the forged piece: when delta<At 200mm,. DELTA.Ti130 ℃ under normal temperature; when delta is more than or equal to 200mm and less than 300mm, delta TiThe temperature is 100 ℃; when delta is more than or equal to 300mm and less than 400mm, delta Ti=80℃;
The calculation mode of the gradual temperature rise times n is as follows:
Figure BDA0003564805560000051
n is an integer; wherein T is a planned heating target temperature, TaThe temperature of the forged piece before temperature rise;
holding time tiThe calculation formula of (2) is as follows: t is ti=(10+2ni) min, wherein niFor the ith heating, ni=i,i=1,2…,n。
The gradual cooling mode in the step (5) is as follows: gradually cooling the forging piece for N times at a cooling speed of less than 50 ℃/h to reduce the temperature to a preset cooling target temperature, wherein the temperature is reduced by delta T each timejAnd is kept for a certain time t after each coolingj
Wherein, Delta TjDetermining according to the wall thickness delta of the forged piece: when delta is less than 200mm, delta TjThe temperature is 200 ℃; when delta is more than or equal to 200mm and less than 300mm, delta Tj150 ℃ is set; when delta is more than or equal to 300mm and less than 400mm, delta Tj=100℃;
The calculation formula of the gradual cooling times N is as follows:
Figure BDA0003564805560000052
taking an integer from N upwards; wherein, TbThe temperature before the temperature reduction of the forge piece is carried out, and T' is the set temperature target temperature;
holding time tjThe calculation formula of (2) is as follows: t is tj=2(10+(N-2nj) Min, wherein n isjFor the j th heating, ni=i,i=1,2…,N。
Example 1
Referring to FIG. 1, 2.25Cr-1Mo-0.25V steel materials are selected according to the regulation and control method to prepare test pieces, wherein the wall thickness is 350mm, the inner diameter is 200mm, and 2 test pieces are prepared. The specific process comprises the following steps:
(1) pretreatment before forging:
rapidly heating the steel ingot to 300 ℃ within 30min, preserving heat for 40min, then heating to 700 ℃ at the heating rate of 45 ℃/h, and preserving heat for 6 h; then heating the steel ingot to 800 ℃ at a heating rate of 30 ℃/h, and preserving heat for 1 h; after the temperature is stable, heating the steel ingot to 900 ℃ at the same heating rate, and preserving the heat for 1.5 h; then raising the temperature to 1000 ℃ at the same temperature raising speed, and preserving the temperature for 2 h; finally, heating to 1180 ℃ at the same heating speed, and preserving heat for 3 hours;
(2) forging and forming:
forging and molding the steel ingot to obtain a forging piece with the wall thickness of 350mm, wherein the final forging temperature is 960 ℃;
(3) pretreatment after forging:
rapidly transferring the forged piece with the initial temperature of 960 ℃ after forging forming to a heat treatment furnace, cooling the forged piece to 700 ℃ at the cooling speed of 20 ℃/h, and preserving heat for 20 h; after the step is finished, continuously performing the following step (4) on one hydrogenation reactor sample, performing air cooling on the other hydrogenation reactor sample, and detecting the residual stress after the temperature is reduced to the room temperature, wherein the surface residual stress is 212MPa, and the core residual stress is 230 MPa;
(4) full thickness tissue-stress-property recovery treatment:
after the heat preservation stage is completed, the temperature of the forge piece is gradually increased to 1050 ℃ at the temperature increasing speed of 30 ℃/h, specifically, the temperature is increased for 5 times, the temperature is increased for 80 ℃ for the first four times, the temperature is increased for 30 ℃ for the last time, the temperature is respectively preserved for 12min, 14min, 16min, 18min and 20min after each time of temperature increase, and then the temperature is preserved for 7.5h at 1050 ℃;
after the temperature preservation at 1050 ℃, the temperature of the forge piece is gradually reduced to 700 ℃ at a cooling speed of 40 ℃/h, specifically, the temperature is reduced for 4 times, the temperature is reduced for 100 ℃ in the first three times, the temperature is reduced for 50 ℃ in the last time, the temperature is respectively preserved for 24min, 20min, 16min and 12min after each time of temperature reduction, and then the temperature is preserved for 16h at 700 ℃;
after the heat preservation at 700 ℃, the forging is continuously cooled to 400 ℃ gradually at a cooling speed of 40 ℃/h, specifically, the temperature is reduced for 3 times, the temperature is reduced for 100 ℃ each time, the temperature is respectively preserved for 22min, 18min and 14min after each time of temperature reduction, and then the forging is naturally cooled to room temperature for rough machining;
after rough machining is finished, rapidly heating to 400 ℃, then gradually heating the forging to 930 ℃ at a heating rate of 30 ℃/h, specifically heating 7 times, wherein the temperature is increased by 80 ℃ for the first six times, and is increased by 50 ℃ for the last time, and after each heating, the temperature is respectively maintained for 12min, 14min, 16min, 18min, 20min, 22min and 24min, and then the temperature is maintained for 10h at 930 ℃;
after the thermal insulation at 930 ℃, transferring the forged piece into a rotary quenching bath, quenching the forged piece at a cooling speed of 5 ℃/h, and cooling to 200 ℃ after quenching;
transferring the quenched forging to a heat treatment furnace, slowly cooling to 150 ℃, and keeping for 5 hours;
then gradually heating the forging piece to 700 ℃ at the heating rate of 30 ℃/h, specifically heating for 7 times, heating for the first 6 times to 80 ℃, heating for the last time to 70 ℃, respectively preserving heat for 12min, 14min, 16min, 18min, 20min, 22min and 24min after each heating, and then preserving heat for 18h at 700 ℃;
and after the heat preservation at 700 ℃, cooling to below 300 ℃ at a cooling speed of 25 ℃/h, and then discharging from the furnace for air cooling to obtain a hydrogenation reactor sample.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that after the forging is finished, the comparative example is directly and rapidly cooled to 300 ℃, then slowly cooled to 200 ℃ and kept warm for 6 hours; then gradually heating up to 1050 ℃ at the heating rate of 30 ℃/h and preserving heat for 7.5h, and the other steps are the same. In addition, 2 test pieces with the wall thickness of 350mm and the inner diameter of 200mm are also arranged in the comparative example 1, one test piece is subjected to the whole heat treatment process according to the method of the comparative example 1, the other test piece is firstly rapidly cooled to 300 ℃ after forging is completed, then is slowly cooled to 200 ℃ and is kept warm for 6 hours, then is air-cooled to room temperature, and the residual stress is detected after the temperature is reduced to the room temperature, wherein the surface residual stress is 320MPa, and the core residual stress is 346 MPa.
The above comparative example 1 is a currently used post-forging treatment method, and is usually subjected to rapid cooling directly after forging and then to heat treatment.
Comparative example 2
The comparative example 2 is provided with 1 test piece with the wall thickness of 350mm and the inner diameter of 200mm, and is different from the example 1 in that the comparative example does not adopt a method of gradually heating up and gradually cooling down in the step of full-thickness structure-stress-performance recovery treatment, only heats up or cools down at a certain speed, and other steps are the same, and the step of full-thickness structure-stress-performance recovery treatment is as follows:
heating the forging to 1050 ℃ at the heating rate of 30 ℃/h, and then preserving heat at 1050 ℃ for 7.5 h;
after the heat preservation at 1050 ℃, cooling the forging to 700 ℃ at the cooling speed of 40 ℃/h, and then preserving the heat for 16h at 700 ℃;
after the heat preservation at 700 ℃, continuously cooling the forging to 400 ℃ at the cooling speed of 40 ℃/h, and then naturally cooling to room temperature for rough machining;
after the rough machining is finished, quickly heating to 400 ℃, then heating the forge piece to 930 ℃ at the heating speed of 30 ℃/h, and then preserving heat at 930 ℃ for 10 h;
after the thermal insulation at 930 ℃, transferring the forged piece into a rotary quenching bath, quenching the forged piece at a cooling speed of 5 ℃/h, and cooling to 200 ℃ after quenching;
transferring the quenched forging to a heat treatment furnace, slowly cooling to 150 ℃, and keeping for 5 hours;
then heating the forging to 700 ℃ at the heating rate of 30 ℃/h, and then preserving heat at 700 ℃ for 18 h;
and after the heat preservation at 700 ℃, cooling to below 300 ℃ at a cooling speed of 25 ℃/h, and then discharging from the furnace for air cooling to obtain a hydrogenation reactor sample.
Comparative example 3
Comparative example 3 1 test piece with a wall thickness of 350mm and an internal diameter of 200mm was provided, which differs from example 1 in that: the pretreatment after forging in the step (3) and the full-thickness structure-stress-performance recovery treatment in the step (4) are different, and other steps are the same.
The post-forging pretreatment procedure in comparative example 3 was: directly and rapidly cooling to 300 ℃, then slowly cooling to 200 ℃ and keeping the temperature for 6 h.
The full thickness structure-stress-performance recovery processing steps in comparison 3 are as follows:
heating the forging to 1050 ℃ at the heating rate of 30 ℃/h, and then preserving heat at 1050 ℃ for 7.5 h;
after the heat preservation at 1050 ℃, cooling the forging to 700 ℃ at the cooling speed of 40 ℃/h, and then preserving the heat for 16h at 700 ℃;
after the heat preservation at 700 ℃, continuously cooling the forging to 400 ℃ at the cooling speed of 40 ℃/h, and then naturally cooling to room temperature for rough machining;
after rough machining is finished, rapidly heating to 400 ℃, then heating the forge piece to 930 ℃ at the heating speed of 30 ℃/h, and then preserving heat for 10h at 930 ℃;
after the thermal insulation at 930 ℃, transferring the forged piece into a rotary quenching bath, quenching the forged piece at a cooling speed of 5 ℃/h, and cooling to 200 ℃ after quenching;
transferring the quenched forging to a heat treatment furnace, slowly cooling to 150 ℃, and keeping for 5 hours;
then heating the forging to 700 ℃ at the heating rate of 30 ℃/h, and then preserving heat at 700 ℃ for 18 h;
and after the heat preservation at 700 ℃, cooling to below 300 ℃ at a cooling speed of 25 ℃/h, and then discharging from the furnace for air cooling to obtain a hydrogenation reactor sample. The full thickness sampling test was performed on the above example 1 and comparative examples 1 to 3, and the test results are shown in table 1. As can be seen from Table 1, the grain size of the product structure can reach 8 grades by the regulating method, the yield strength and the tensile strength are high, and particularly, the residual stress is low, which indicates that the heat preservation at about 700 ℃ after forging not only has the effects of grain refinement and product performance improvement, but also has a good residual stress eliminating effect; meanwhile, the invention adopts the modes of gradually heating and gradually cooling in the heating and cooling stages, so that the structure, the stress and the performance in the full thickness direction are uniform and consistent.
TABLE 1 Performance test data
Figure BDA0003564805560000081
The parts which are not described in the invention can be realized by adopting or referring to the prior art.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.

Claims (5)

1. The method for regulating and controlling the whole-thickness structure-stress-performance uniformity of the ultra-thick forging of the large hydrogenation reactor is characterized by comprising the following steps of:
(1) rapidly heating the steel ingot to 300-350 ℃, then heating to 650-700 ℃ at a heating rate not more than 56 ℃/h, and preserving heat for 4-6 h; then, heating the steel ingot to 1180 +/-10 ℃ in sections, and preserving heat for 2-4 hours;
(2) forging and forming the steel ingot within the steel ingot forging temperature range in the step (1), and controlling the forging final temperature to be not less than 850 ℃;
(3) after the forging in the step (2) is completed, transferring the forged piece to a heat treatment furnace, cooling the forged piece to 700 +/-10 ℃ at a cooling speed of 20-30 ℃/h, and preserving heat for 15-20 h to ensure that the grain size of the forged piece reaches 6 grades or above and the residual stress is reduced to 200-260 MPa;
(4) on the basis of the step (3), heating to 1040-1080 ℃ in a gradual heating manner, and keeping for a certain time t1
(5) Cooling to 660-720 ℃ in a gradual cooling way and keeping for a certain time t2(ii) a Then gradually cooling to 350-400 ℃, and naturally cooling to room temperature for rough machining;
(6) after rough machining is finished, quickly heating to 400 ℃, then heating to 920-950 ℃ in a gradual heating mode, and keeping for a certain time t3(ii) a Then transferring the forged piece to a quenching bath, quenching the forged piece at a cooling speed of not less than 5 ℃/h, and cooling to 200-250 ℃ after quenching so that the structural components of the forged piece in the full thickness direction are lower bainite;
(7) transferring the quenched forge piece to a heat treatment furnace, slowly cooling to 150 +/-10 ℃, and keeping for 3-6 hours; then gradually heating to 660-720 ℃, and keeping for a certain time t4(ii) a Finally cooling to below 300 ℃ at a cooling speed of 20-30 ℃/h, and dischargingAnd (5) performing air cooling in the furnace to reduce the residual stress of the forging in the full thickness direction to be less than 100 MPa.
Said t is1=(0.01δ+4)h,t2=(0.04δ+2)h,t3=(0.02δ+3)h,t4δ is the forging wall thickness in mm (0.02 δ +10) h.
2. The method for regulating and controlling the whole-thickness structure-stress-performance uniformity of the ultra-thick forging of the large-scale hydrogenation reactor according to claim 1, wherein the step (1) comprises the following steps: heating the steel ingot to 800 +/-20 ℃ at a heating rate of less than 45 ℃/h, and preserving heat for 1-2 h; after the temperature is stable, heating the steel ingot to 900 +/-20 ℃ at the same heating speed, and preserving the heat for 1-2 hours; then, heating to 1000 +/-20 ℃ at the same heating rate, and preserving heat for 1-2 h; and finally, heating to 1180 +/-10 ℃ at the same heating speed, and preserving heat for 2-4 hours.
3. The method for regulating and controlling the whole-thickness structure-stress-performance uniformity of the ultra-thick forged piece of the large-sized hydrogenation reactor according to claim 1, wherein in the step (2), the temperature of the forged piece is controlled to be not less than 850 ℃ in the forging process, and if the temperature is less than 850 ℃, the temperature needs to be raised to 1180 +/-10 ℃ in a furnace, and the temperature is kept for 1-2 hours.
4. The method for regulating and controlling the whole-thickness structure-stress-performance uniformity of the ultra-thick forging of the large-scale hydrogenation reactor according to claim 1, wherein the gradual temperature rise in the steps (4), (6) and (7) is as follows: gradually heating the forging piece at a heating rate of not more than 35 ℃/h for n times to raise the temperature to a preset heating target temperature, wherein the temperature is raised by delta T every timeiKeeping the temperature at a certain value for a certain time t after each temperature risei
Wherein, Delta TiDetermining according to the wall thickness delta of the forged piece: when delta<At 200mm,. DELTA.Ti130 deg.C; when delta is more than or equal to 200mm and less than 300mm, delta TiAt 100 deg.C; when delta is more than or equal to 300mm and less than 400mm, delta Ti=80℃;
The calculation mode of the gradual temperature rise times n is as follows:
Figure FDA0003564805550000021
n is an integer upwards; wherein T is a planned heating target temperature, TaThe temperature of the forged piece before temperature rise;
holding time tiThe calculation formula of (2) is as follows: t is ti=(10+2ni) min, wherein niFor the ith heating, ni=i,i=1,2…,n。
5. The method for regulating and controlling the whole-thickness structure-stress-performance uniformity of the ultra-thick forging of the large-scale hydrogenation reactor according to claim 1, wherein the gradual cooling mode in the step (5) is as follows: gradually cooling the forging piece for N times at a cooling speed of less than 50 ℃/h to reduce the temperature to a preset cooling target temperature, wherein the temperature is reduced by delta T each timejAnd is kept for a certain time t after each coolingj
Wherein, Delta TjDetermining according to the wall thickness delta of the forged piece: when delta is less than 200mm, delta TjThe temperature is 200 ℃; when delta is more than or equal to 200mm and less than 300mm, delta Tj150 ℃ is set; when delta is more than or equal to 300mm and less than 400mm, delta Tj=100℃;
The calculation formula of the gradual cooling times N is as follows:
Figure FDA0003564805550000022
taking an integer from N upwards; wherein, TbThe temperature before the temperature reduction of the forge piece is carried out, and T' is the set temperature target temperature;
holding time tjThe calculation formula of (2) is as follows: t is tj=2(10+(N-2nj) Min, wherein njFor the j th heating, ni=i,i=1,2…,N。
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