CN115896784A - Cobalt removing device and cobalt removing method for diamond composite sheet - Google Patents
Cobalt removing device and cobalt removing method for diamond composite sheet Download PDFInfo
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- CN115896784A CN115896784A CN202211618604.3A CN202211618604A CN115896784A CN 115896784 A CN115896784 A CN 115896784A CN 202211618604 A CN202211618604 A CN 202211618604A CN 115896784 A CN115896784 A CN 115896784A
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Abstract
The invention discloses a cobalt removing device for a diamond composite sheet, which comprises a bracket, a cobalt removing reagent storage barrel and a cobalt removing reaction barrel, wherein the bottom end port of the cobalt removing reagent storage barrel is connected with the upper end port of the cobalt removing reaction barrel through a middle valve, the upper end port of the cobalt removing reagent storage barrel is provided with a storage barrel bottom cover, the bottom end wall of the cobalt removing reagent storage barrel is provided with a cobalt removing reagent inlet and a cobalt removing reagent outlet, the side wall of the cobalt removing reaction barrel is provided with a cobalt removing hole, the upper end of the cobalt removing reaction barrel is provided with a deionized water inlet and a deionized water outlet, a corrosion-resistant filler block is arranged in the cobalt removing reaction barrel, the bottom of the cobalt removing reaction barrel is provided with a heating pipe and a reaction barrel bottom cover, and the reaction barrel bottom cover is provided with a heating liquid inlet and a heating liquid outlet. The invention has the beneficial effects that: this cobalt device is taken off to diamond compact piece, the operation is safe high-efficient, promotes and takes off cobalt efficiency, prevents polluted environment and bodily injury simultaneously, is applicable to the enterprise's production.
Description
Technical Field
The invention relates to the technical field of material decobalting, in particular to a decobalting device and a decobalting method for a diamond compact.
Background
The common sintering aid for PDC is cobalt, and during the high-temperature and high-pressure sintering process, the cobalt promotes a large amount of diamond-diamond grains to directly form bonds (D-D bonds), so that the PDC has higher strength and wear resistance. The PDC works under high temperature and high stress conditions, and because the coefficient of thermal expansion of cobalt and diamond is greatly different, diamond grains in a diamond layer are easy to fall off in the working process, so that the service performance of the PDC can be reduced. In addition, when the temperature is higher than 700 ℃, the metal cobalt can catalyze the diamond to generate reverse transformation to the graphite, so that the hardness and the wear resistance of the PDC are sharply reduced. Therefore, the cobalt in the PDC diamond layer is removed, and the thermal stability of the PDC can be greatly improved.
Based on the above, it is necessary to perform the cobalt removal treatment of the PDC. But the 'neck clamp' problem mainly exists at present: 1) The PDC decobalting efficiency is low, so that the product supply period is long, the cost is high, and the order delivery period is influenced; 2) Aiming at different PDC products, the cobalt removal rate is inconsistent, the thermal stability of the PDC products with low cobalt removal rate is relatively poor, and low-end PDC products with high proportion appear; 3) Can not meet the customer requirements of the PDC products with higher cobalt removal depth. Initial experiments show that the decobalting depth increases but the decobalting speed gradually decreases with the lengthening of the decobalting time.
The prior PDC cobalt removal technology generally adopts corrosive strong acid or a mixed solution of a plurality of strong acids as a cobalt removal reagent, and the strong corrosivity of the strong acid reagent is utilized to achieve the cobalt removal effect, but the cobalt removal efficiency is general, and the basal part is easy to corrode. Meanwhile, the use of part of strong acid reagents, such as nitric acid and hydrofluoric acid, has high danger and causes pollution to the environment.
Disclosure of Invention
The invention aims to provide a cobalt removing device and a cobalt removing method for a diamond compact, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a diamond compact piece takes off cobalt device, includes the support, takes off the cobalt reagent and stores the bucket and take off cobalt reaction barrel, take off the cobalt reagent store the bottom mouth of bucket with take off cobalt reaction barrel upper port and connect through middle valve, the upper port that takes off the cobalt reagent and store the bucket is equipped with and stores the barrel head, the bottom wall that takes off the cobalt reagent and store the bucket is equipped with takes off cobalt reagent entry and takes off cobalt reagent export, it is provided with and takes off the cobalt hole to take off cobalt reaction barrel lateral wall, it sets up deionized water entry and deionized water export to take off cobalt reaction barrel upper end, it sets up corrosion-resistant filler block to take off cobalt reaction barrel inside, it is provided with heating pipe and reaction barrel head to take off cobalt reaction barrel head portion, the reaction barrel head is provided with heating fluid entry and heating fluid export.
Preferably, it is downthehole to take off the cobalt is equipped with the diamond compact piece protection frock, the diamond compact piece protection frock is close to the one end of taking off the cobalt reaction barrel is equipped with the diamond compact piece, the diamond compact piece protection frock is kept away from the one end of taking off the cobalt reaction barrel is equipped with the exhaust hole.
Preferably, the number of the cobalt removing holes is several, and the several cobalt removing holes are uniformly distributed on the side wall of the cobalt removing reaction barrel.
Preferably, the periphery be equipped with the annular sleeve, annular sleeve decobalt reaction barrel integrated into one piece, the annular cover lead to with compound piece protection frock threaded connection.
Preferably, a sealing gasket is arranged between the cobalt removing hole and the diamond compact protection tool.
Preferably, a bearing is arranged in the middle of the support frame, and the support frame is connected with a wall or a fixed support frame through the bearing.
Preferably, the heating pipe is arranged at the bottom end of the inner cavity of the cobalt removal reaction barrel, and the heating pipe is annularly arranged and is at least one circle to many circles.
Preferably, the inner cavity wall surfaces of the cobalt-removing reagent storage barrel and the cobalt-removing reaction barrel are both provided with high-temperature-resistant and corrosion-resistant coatings, and the shapes of the cobalt-removing reagent storage barrel and the cobalt-removing reaction barrel include, but are not limited to, a round barrel and a square barrel.
A cobalt removing method for a diamond compact of a cobalt removing device for the diamond compact comprises the following steps:
s1, closing an intermediate valve, and closing valves of a cobalt removal reagent inlet, a cobalt removal reagent outlet, a deionized water inlet and a deionized water outlet;
s2, opening a cobalt removal reagent inlet valve, injecting a proper cobalt removal reagent from a cobalt removal reagent inlet, and then closing the cobalt removal reagent inlet valve;
s3, placing the diamond composite sheet into a composite sheet protection tool, sleeving a sealing pad on the composite sheet protection tool, and screwing the composite sheet protection tool into the corresponding cobalt removing hole;
and S4, checking and confirming the air tightness of the cobalt removal reagent storage barrel and the cobalt removal reaction barrel by observing the numerical value of the barometer.
S5, on the premise of confirming good air tightness, opening an intermediate valve to enable a cobalt removal reagent to flow into a cobalt removal reaction barrel, and simultaneously injecting a heating liquid with a certain temperature into a heating liquid inlet to ensure continuous circulation in a heating pipe;
s6, the diamond composite sheet starts to undergo a cobalt removal process, the air tightness of the cobalt removal reaction barrel is continuously kept, and an intermediate valve is opened to supplement a cobalt removal reagent every other day;
s7, after the cobalt removal process of the diamond composite sheet is finished, firstly closing a heating liquid inlet, then opening an intermediate valve, finally turning over the support frame by 180 degrees through a bearing in the middle of the support frame to enable the cobalt removal reagent to return to a cobalt removal reagent storage barrel, and closing the intermediate valve;
s8, injecting deionized water from a deionized water inlet, and allowing the deionized water with the residual cobalt removal reagent to flow out from a deionized water outlet;
s9, detaching the composite sheet protection tool and the diamond composite sheet;
and S10, a bearing is arranged in the center of the support frame, the support frame is turned over by 180 degrees, a valve of a cobalt removal reagent outlet is opened, a cobalt removal reagent in the cobalt removal reagent storage barrel flows into a cobalt removal reagent storage place from the cobalt removal reagent outlet for standby, and cobalt removal is completed.
Preferably, the decobalting reagent comprises: hydrochloric acid, sulfuric acid, perchloric acid, iron acetate, citric acid and deionized water, wherein the mass ratio of (1-10): 1-5:1-3:1-20.
Compared with the prior art, the invention has the beneficial effects that: the cobalt removing device for the diamond composite sheet is safe and efficient to operate, improves the cobalt removing efficiency, prevents environmental pollution and personal injury, is suitable for enterprise production, and is embodied in the following points:
1. the decobalting reagent adopts a relatively safe reagent, and a strong toxic reagent such as hydrofluoric acid is abandoned;
2. the cobalt removal reagent storage barrel and the cobalt removal reaction barrel are separately designed, firstly, the cobalt removal reagent can be supplemented as required under the condition of not opening equipment, and then, a deionized water cleaning step is added. The contact of workers to the cobalt removal reagent is avoided to the maximum extent, and the safety is further improved;
3. the design of the vent hole in the protective tool for the composite sheet is beneficial to smooth discharge of gas generated in the cobalt removal process of the diamond composite sheet, the phenomenon that the sealing gasket is opened due to excessive gas is avoided, further the corrosion of a cobalt removal reagent on a diamond composite sheet substrate is avoided, and meanwhile, the air tightness of the cobalt removal device is ensured;
4. the design of the heating oil pipe provides necessary temperature for the cobalt removal process. The air tightness of the whole cobalt removing device ensures the pressure of the cobalt removing process;
5. the design of the corrosion-resistant filler block reduces the usage amount of the cobalt removal reagent and reduces the cost.
Drawings
FIG. 1 is a schematic view of the structure of the present invention;
FIG. 2 is a schematic side sectional view of the present invention;
fig. 3 is an enlarged view of a portion a in fig. 2.
In the figure: 1. a support frame; 2. a storage barrel bottom cover; 3. a cobalt removal reagent storage barrel; 4. a cobalt removal reagent inlet; 5. a cobalt removal reagent outlet; 6. an intermediate valve; 7. a deionized water inlet; 8. a deionized water outlet; 9. a cobalt removal reaction barrel; 10. a corrosion resistant filler block; 11. protecting the tool by using the composite sheet; 12. a diamond compact; 13. a heating fluid inlet; 14. a heating fluid outlet; 15. a bottom cover of the reaction barrel; 16. a gasket; 17. heating a tube; 18. an exhaust hole; 19. an annular sleeve; 20. a barometer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1-3, the present invention provides a technical solution: the utility model provides a diamond compact piece takes off cobalt device, includes support 1, takes off the cobalt reagent and stores bucket 3 and take off cobalt reaction bucket 9, take off the cobalt reagent store bucket 3 the bottom mouth with take off cobalt reaction bucket 9 upper end mouth and connect through middle valve 6, the upper end mouth that takes off cobalt reagent and store bucket 3 is equipped with and stores bucket bottom 2, the bottom wall that takes off cobalt reagent and store bucket 3 is equipped with takes off cobalt reagent entry 4 and takes off cobalt reagent export 5, it is provided with and takes off the cobalt hole to take off cobalt reaction bucket 9 lateral wall, it sets up deionized water entry 7 and deionized water export 8 to take off cobalt reaction bucket 9 upper ends, it sets up corrosion-resistant filler block 10 to take off cobalt reaction bucket 9 inside, it is provided with heating pipe 17 and reaction bucket bottom 15 to take off cobalt reaction bucket 9 bottom, reaction bucket bottom 15 is provided with heating fluid entry 13 and heating fluid export 14.
Specifically, it is downthehole to take off cobalt is equipped with diamond compact piece protection frock 11, diamond compact piece protection frock 11 is close to take off cobalt reaction barrel 9's one end is equipped with diamond compact piece 12, diamond compact piece protection frock 11 is kept away from take off cobalt reaction barrel 9's one end and be equipped with exhaust hole 18.
Specifically, the number of the cobalt removing holes is several, and the several cobalt removing holes are uniformly distributed on the side wall of the cobalt removing reaction barrel 9.
Specifically, the periphery be equipped with annular sleeve 19, annular sleeve 19 takes off cobalt reaction barrel 9 integrated into one piece, annular set through 19 with compound piece protection frock 11 threaded connection.
Specifically, a sealing gasket 16 is arranged between the cobalt removing hole and the diamond compact protection tool 11.
Specifically, the middle of the support frame 1 is provided with a bearing, and the support frame 1 is connected with a wall or a fixed support frame through the bearing.
Specifically, the heating pipe 17 is arranged at the bottom end of the inner cavity of the cobalt-removing reaction barrel 9, and the heating pipe 17 is annularly arranged and is arranged in one circle or more circles.
Specifically, the inner cavity wall surfaces of the cobalt removal reagent storage barrel 3 and the cobalt removal reaction barrel 9 are both provided with high temperature resistant and corrosion resistant coatings, and the shapes of the cobalt removal reagent storage barrel and the cobalt removal reaction barrel include but are not limited to a round barrel and a square barrel.
Example two
The embodiment provides a cobalt removing method for a diamond compact, which comprises the following steps:
s1, closing an intermediate valve 6, and closing valves of a cobalt removal reagent inlet 4, a cobalt removal reagent outlet 5, a deionized water inlet 7 and a deionized water outlet 8;
s2, opening a valve of a cobalt removal reagent inlet 4, and closing the valve of the cobalt removal reagent inlet 4 after injecting a proper cobalt removal reagent from the cobalt removal reagent inlet 4;
s3, placing the diamond composite sheet 12 into the composite sheet protection tool 11, sleeving the composite sheet protection tool 11 on the sealing gasket 16, and screwing the composite sheet protection tool into the corresponding cobalt removing hole;
and S4, checking and confirming the airtightness of the cobalt removal reagent storage barrel 3 and the cobalt removal reaction barrel 9 by observing the value of the barometer 20.
S5, on the premise of confirming that the air tightness is good, opening an intermediate valve 6 to enable a cobalt removal reagent to flow into a cobalt removal reaction barrel 9, simultaneously injecting heating liquid with a certain temperature into a heating liquid inlet 13, and ensuring continuous circulation in a heating pipe 17;
s6, the diamond composite sheet 12 starts to go through the cobalt removal process, the air tightness of the cobalt removal reaction barrel 9 is continuously kept, and the middle valve 6 is opened to supplement a cobalt removal reagent every 3-15 days;
s7, after the cobalt removal process of the diamond composite sheet 12 is finished, firstly closing the heating liquid inlet 13, then opening the intermediate valve 6, finally turning the support frame 1 by 180 degrees through a bearing in the middle of the support frame 1 to enable the cobalt removal reagent to return to the cobalt removal reagent storage barrel 3, and closing the intermediate valve 6;
s8, injecting deionized water from the deionized water inlet 7, and allowing the deionized water with the residual cobalt removal reagent to flow out from the deionized water outlet 8;
s9, unloading the composite sheet protection tool 11 and the diamond composite sheet 12;
and S10, a bearing is arranged in the center of the support frame 1, the support frame 1 is turned over by 180 degrees, a valve of the cobalt removal reagent outlet 5 is opened, the cobalt removal reagent in the cobalt removal reagent storage barrel 3 flows into a cobalt removal reagent storage place from the cobalt removal reagent outlet 5 for standby, and cobalt removal is completed.
10. The method for decobalting a diamond compact of a decobalting apparatus of a diamond compact of claim 9, wherein: the cobalt removing reagent comprises: hydrochloric acid, sulfuric acid, perchloric acid, iron acetate and citric acid deionized water, wherein the mass ratio of (1-10): 1-5:1-3:1-20.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The utility model provides a cobalt device is taken off to diamond compact which characterized in that: including support (1), take off cobalt reagent and store bucket (3) and take off cobalt reaction barrel (9), take off cobalt reagent store the bottom mouth of bucket (3) with take off cobalt reaction barrel (9) upper port and pass through intermediate valve (6) and connect, the last port that takes off cobalt reagent and store bucket (3) is equipped with stores barrel head (2), the bottom wall that takes off cobalt reagent and store bucket (3) is equipped with takes off cobalt reagent entry (4) and takes off cobalt reagent export (5), it is provided with the cobalt hole to take off cobalt reaction barrel (9) lateral wall, it sets up deionized water entry (7) and deionized water export (8) to take off cobalt reaction barrel (9) upper end, take off cobalt reaction barrel (9) inside and set up corrosion-resistant filler block (10), it is provided with heating pipe (17) and reaction barrel head (15) to take off cobalt reaction barrel (9) bottom, reaction barrel head (15) are provided with heating fluid entry (13) and heating fluid export (14).
2. The apparatus of claim 1, wherein: it is downthehole to take off cobalt is equipped with diamond compact piece protection frock (11), diamond compact piece protection frock (11) are close to the one end of taking off cobalt reaction barrel (9) is equipped with diamond compact piece (12), diamond compact piece protection frock (11) are kept away from the one end of taking off cobalt reaction barrel (9) is equipped with exhaust hole (18).
3. The device and the method for removing cobalt from a diamond compact according to claim 2, wherein: the number of the cobalt removing holes is a plurality, and the plurality of the cobalt removing holes are uniformly distributed on the side wall of the cobalt removing reaction barrel (9).
4. The device and the method for removing cobalt from a diamond compact according to claim 3, wherein: the periphery be equipped with annular sleeve (19), annular sleeve (19) take off cobalt reaction barrel (9) integrated into one piece, annular set lead to (19) with compound piece protection frock 11 threaded connection.
5. The device and the method for removing cobalt from the diamond compact according to claim 4, wherein: be equipped with sealed pad (16) between the cobalt hole of taking off with diamond compact piece protection frock (11).
6. The apparatus and method for decobalting a diamond compact according to claim 5, wherein: the support frame is characterized in that a bearing is arranged in the middle of the support frame (1), and the support frame (1) is connected with a wall or a fixed support frame through the bearing.
7. The cobalt removing device and the cobalt removing method for the diamond compact as claimed in claim 6, wherein: the heating pipe (17) is arranged at the bottom end of the inner cavity of the cobalt-removing reaction barrel (9), and the heating pipe (17) is annularly arranged and is arranged in one circle or more circles.
8. The apparatus and method for decobalting a diamond compact according to claim 7, wherein: the inner cavity wall surfaces of the cobalt-removing reagent storage barrel (3) and the cobalt-removing reaction barrel (9) are respectively provided with a high-temperature-resistant and corrosion-resistant coating, and the shapes of the cobalt-removing reagent storage barrel (3) and the cobalt-removing reaction barrel (9) include but are not limited to a round barrel and a square barrel.
9. A method for removing cobalt from a diamond compact based on the apparatus for removing cobalt from a diamond compact according to any one of claims 1 to 9, comprising: the method comprises the following steps:
s1, closing an intermediate valve (6), and closing valves of a decobalting reagent inlet (4), a decobalting reagent outlet (5), a deionized water inlet (7) and a deionized water outlet (8);
s2, opening a valve of a cobalt removal reagent inlet (4), injecting a proper cobalt removal reagent from the cobalt removal reagent inlet (4), and closing the valve of the cobalt removal reagent inlet (4);
s3, placing the diamond composite sheet (12) into a composite sheet protection tool (11), sleeving a sealing gasket (16) on the composite sheet protection tool (11), and screwing the composite sheet protection tool into the corresponding cobalt removing hole;
and S4, checking and confirming the airtightness of the cobalt removal reagent storage barrel (3) and the cobalt removal reaction barrel (9) by observing the value of the barometer (20).
S5, on the premise of confirming good air tightness, opening an intermediate valve (6) to enable a cobalt removal reagent to flow into a cobalt removal reaction barrel (9), simultaneously injecting a heating liquid with a certain temperature into a heating liquid inlet (13), and ensuring continuous circulation in a heating pipe (17);
s6, the diamond composite sheet (12) starts to undergo a cobalt removal process, the air tightness of the cobalt removal reaction barrel (9) is continuously kept, and the middle valve (6) is opened to supplement a cobalt removal reagent every 3-15 days;
s7, after the cobalt removal process is finished by the diamond composite sheet (12), firstly closing a heating liquid inlet (13), then opening an intermediate valve (6), finally turning over the support frame (1) by 180 degrees through a bearing in the middle of the support frame (1) to return a cobalt removal reagent to a cobalt removal reagent storage barrel (3), and closing the intermediate valve (6);
s8, injecting deionized water from a deionized water inlet (7), and allowing the deionized water with the residual cobalt removal reagent to flow out from a deionized water outlet (8);
s9, unloading the composite sheet protection tool (11) and the diamond composite sheet (12);
s10, a bearing is arranged in the center of the support frame (1), the support frame (1) is turned over by 180 degrees, a valve of the cobalt removal reagent outlet (5) is opened, the cobalt removal reagent in the cobalt removal reagent storage barrel (3) flows into a cobalt removal reagent storage place for later use through the cobalt removal reagent outlet (5), and cobalt removal is completed.
10. The method for decobalting a diamond compact of a decobalting apparatus of a diamond compact of claim 9, wherein: the cobalt removing reagent comprises: hydrochloric acid, sulfuric acid, perchloric acid, iron acetate, citric acid and deionized water, wherein the mass ratio of (1-10) to (1-10): (1-5): (1-3): (1-20).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211618604.3A CN115896784B (en) | 2022-12-15 | 2022-12-15 | Cobalt removing device and cobalt removing method for diamond compact |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211618604.3A CN115896784B (en) | 2022-12-15 | 2022-12-15 | Cobalt removing device and cobalt removing method for diamond compact |
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| CN115896784A true CN115896784A (en) | 2023-04-04 |
| CN115896784B CN115896784B (en) | 2024-08-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN119220978A (en) * | 2024-12-02 | 2024-12-31 | 河南晶研智造科技有限公司 | A cobalt removal device for polycrystalline diamond composite sheet and a cobalt removal method using the device |
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| CN119220978A (en) * | 2024-12-02 | 2024-12-31 | 河南晶研智造科技有限公司 | A cobalt removal device for polycrystalline diamond composite sheet and a cobalt removal method using the device |
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