CN115921880A - Preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomer - Google Patents
Preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomer Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 65
- 239000003054 catalyst Substances 0.000 title claims abstract description 29
- 229910002058 ternary alloy Inorganic materials 0.000 title claims abstract description 28
- 239000000178 monomer Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 13
- 239000010703 silicon Substances 0.000 title claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000009792 diffusion process Methods 0.000 claims abstract description 32
- 229910052802 copper Inorganic materials 0.000 claims abstract description 25
- 239000010949 copper Substances 0.000 claims abstract description 25
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- 239000011812 mixed powder Substances 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 16
- 239000000956 alloy Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 6
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- 238000009692 water atomization Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 238000003860 storage Methods 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 21
- 230000005540 biological transmission Effects 0.000 claims description 20
- 238000007789 sealing Methods 0.000 claims description 20
- 230000001681 protective effect Effects 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 13
- 230000000903 blocking effect Effects 0.000 claims description 11
- 238000003723 Smelting Methods 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 7
- 241000883990 Flabellum Species 0.000 claims description 6
- 238000013016 damping Methods 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
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- 230000000149 penetrating effect Effects 0.000 claims 2
- 238000010521 absorption reaction Methods 0.000 claims 1
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- 238000004519 manufacturing process Methods 0.000 description 15
- 238000000926 separation method Methods 0.000 description 14
- 238000001514 detection method Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
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- 238000009826 distribution Methods 0.000 description 2
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- 239000000376 reactant Substances 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007036 catalytic synthesis reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention provides a preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomers, which comprises the steps of firstly putting electrolytic copper, a standard zinc ingot and an aluminum ingot into a melting furnace for melting, wherein the aluminum ingot and the zinc ingot are firstly added, charcoal is adopted for covering, then the electrolytic copper is added, and when the temperature is raised to 700 ℃, a water atomization process is adopted for preparing CuZnAl precursor powder; adding pure copper powder into the prepared CuZnAl precursor powder, and uniformly mixing by adopting a mixer. Then sending the powder into a diffusion furnace for diffusion treatment, raising the temperature of the furnace to 650 ℃, and then performing diffusion treatment on the mixed powder for 3 hours under the temperature condition; and (3) crushing the obtained CuZnAl alloy powder, and then performing ball milling on the powder in a high-energy ball mill filled with nitrogen to obtain flaky nano CuZnAl ternary alloy catalyst powder.
Description
Technical Field
The invention relates to the technical field of organosilicon monomer synthesis, in particular to a preparation method of CuZnAl ternary alloy catalyst powder for organosilicon monomer synthesis.
Background
The CuZnAl ternary alloy catalyst is flaky copper alloy powder which takes copper as a matrix and takes 10 to 30 weight percent of zinc and 10 to 30 weight percent of aluminum as main additive elements. At present, cuZn, cuAl or simple substance zinc powder, simple substance aluminum powder and simple substance copper powder are mainly used in the synthesis process of the organic silicon monomer, and are matched as auxiliary agents to adjust the catalytic synthesis process of the synthesis reaction of the organic silicon monomer.
The existing diffusion furnace has uneven gas distribution, so that materials are heated unevenly during production, and the product quality is influenced. In addition, the working temperature of the diffusion furnace is extremely high, and workers face high-temperature threats during material taking and placing operation, so that burn accidents are easy to happen once the materials are carelessly operated.
Disclosure of Invention
The invention aims to solve the technical problems that the powder has inconsistent specific gravity, the sedimentation rate of the powder has deviation in the catalysis process, certain waste is caused, and meanwhile, the zinc powder and the aluminum powder are dangerous goods, are inflammable and have larger operation difficulty; meanwhile, the existing diffusion furnace has the problems of uneven gas distribution, influence on the uniformity of product heating during production and reduction of product yield; and the material in the diffusion furnace is inconvenient to take and place.
In order to solve the technical problem, the invention provides a preparation method of CuZnAl ternary alloy catalyst powder for synthesizing an organic silicon monomer, which comprises the following steps:
1) Firstly, putting electrolytic copper, a standard zinc ingot and a standard aluminum ingot into a melting furnace for melting according to the mass part ratio of 10: 4-6; firstly, adding an aluminum ingot and a zinc ingot into a smelting furnace, covering the aluminum ingot and the zinc ingot with charcoal, and then adding electrolytic copper; when the smelting temperature is 700 ℃, precursor powder is prepared by adopting a water atomization process, and the atomization pressure is not less than 20MPa;
2) Adding 2-5 parts of pure copper powder into the precursor powder, and adjusting the chemical components until the ratio of the precursor powder to the pure copper powder is 10 parts: 1-3 parts of CuZnAl and copper mixed powder is prepared by uniformly mixing the components by a mixer;
3) Sending the mixed powder of CuZnAl and copper into a diffusion furnace for diffusion treatment, wherein the furnace temperature is 650 ℃, and then performing diffusion treatment on the mixed powder for 2 to 4 hours under the temperature condition;
4) Crushing the CuZnAl alloy product obtained after diffusion to obtain CuZnAl alloy powder;
5) Screening the crushed CuZnAl alloy powder by using a 150-micron screen, and taking undersize;
6) And adding the crushed powder into a high-energy ball mill filled with nitrogen, and carrying out ball milling to obtain the flaky nano CuZnAl ternary alloy catalyst powder.
Preferably, in the step 1), the particle size of the atomized powder is less than 45um.
Preferably, in the step 2), the pure copper powder is atomized copper powder, and the purity is not lower than 99.6%.
Preferably, the pulverizer in the step 4) is a universal pulverizer, and the high-energy ball mill in the step 5) is a dry ball mill; the rotating speed is not lower than 300r/min, and the purity of the nitrogen is not lower than 99.999 percent.
Preferably, diffusion furnace includes the bottom plate in the step, bottom plate up end fixedly connected with protective structure, protective structure up end fixedly connected with roof, the terminal surface symmetry articulates before the protective structure has sealing door, two terminal surface middle part fixedly connected with exhaust structure before the sealing door, bottom plate up end middle part is provided with shock-absorbing structure, shock-absorbing structure up end fixedly connected with storage structure, the even slip joint of storage structure inner chamber has reaction structure, protective structure inner chamber rear end fixedly connected with separation structure, the equal fixedly connected with separation structure in terminal surface four corners under the bottom plate, terminal surface fixedly connected with rack under the bottom plate, rack up end middle part fixedly connected with drive structure, rack up end front portion is provided with transmission structure, transmission structure up end fixedly connected with elevation structure, elevation structure rear end symmetry fixedly connected with gets the material structure.
Preferably, protective structure includes the guard plate of fixed connection at the bottom plate up end, guard plate rear end face middle part fixedly connected with air inlet, and shock-absorbing structure fixed connection is at the terminal surface middle part under the guard plate inner chamber, sealing door is including articulating the closing plate in the front of the guard plate terminal surface both sides, and the closing plate up end rotates the one end that is connected with pneumatic telescopic rod, and the pneumatic telescopic rod other end rotates with the roof up end to be connected.
Preferably, exhaust structure includes the exhaust frame of fixed connection at the front end face middle part of sealing door, and the even rotation in exhaust frame inner chamber left side is connected with sealed grid, exhaust frame inner chamber symmetry fixedly connected with exhaust frame, and the rotation axis is connected in the rotation of exhaust frame inner chamber, rotation axis inner chamber fixedly connected with micro motor, the even fixedly connected with flabellum of axis of rotation surface, micro motor output and flabellum fixed connection.
Preferably, shock-absorbing structure includes the slide bar of symmetry fixed connection in guard plate inner chamber lower part, and the spring has been cup jointed in the activity of slide bar surface, and slide bar surface symmetry sliding connection has the slider, the spring both ends respectively with two slider fixed connection, the slider up end rotates the one end that is connected with the dwang through the rotating turret, the dwang other end places the board through another rotating turret fixed connection, places board up end fixedly connected with storage structure, places terminal surface middle part fixedly connected with telescopic link under the board, terminal surface and bottom plate fixed connection under the telescopic link.
Preferably, the storage structure includes that fixed connection is at the bracing piece of placing board up end four corners, the even fixedly connected with standing groove of the adjacent one side inner chamber of bracing piece, bracing piece up end fixedly connected with guard plate, standing groove inner chamber slip joint has reaction structure.
Preferably, reaction structure includes the storage board of slide joint at the standing groove inner chamber, and the terminal surface evenly runs through fixedly connected with gas transmission groove before the storage board, and the even fixed connection reaction groove of storage board up end, gas transmission groove run through the reaction groove, the separation structure includes the separation frame of fixed connection at guard plate inner chamber rear portion, and separation frame up end and roof fixed connection, separation frame inner chamber rear end face fixedly connected with connecting plate, connecting plate rear end face fixedly connected with separation board, separation board and air inlet match each other.
Preferably, control panel includes the control panel of fixed connection on guard plate rear end face left side upper portion, and the even fixedly connected with control button in terminal surface lower part before the control panel on terminal surface upper portion fixedly connected with display before the control panel.
Preferably, the heater circuit is communicated with the protection plate and is electrically connected with a control panel of the controller, and the micro motor in the inner cavity of the exhaust structure is communicated with the micro motor and is electrically connected with the protection plate and the control panel in the controller.
Preferably, one side of the side part of the inner cavity of the protection plate is fixedly connected with a temperature detection structure, and the temperature detection structure is electrically connected with the control panel.
Preferably, the driving structure comprises a driving motor fixedly connected to the middle of the upper end face of the placement frame, the output end of the driving motor is fixedly connected with a belt pulley, the outer surface of the belt pulley is in transmission connection with one end of a belt, one end of the belt is in transmission connection with another belt pulley, and the other end of the belt is fixedly connected with the driving structure.
Preferably, the transmission structure includes that the symmetry rotates the gear of connection at the anterior part of rack up end, and the gear rear portion is provided with and places the board and rotate and be connected with the dwang, and dwang surface both sides all are provided with opposite direction's screw thread, dwang surface screw thread and gear intermeshing, dwang surface middle part fixedly connected with the belt pulley, gear up end fixedly connected with elevation structure.
Preferably, elevation structure includes the threaded rod of fixed connection at the gear up end, and the equal threaded connection in threaded rod surface has the elevator, the adjacent one side middle part fixedly connected with gag lever post of elevator, the equal fixedly connected with of elevator rear end face gets the material structure.
Preferably, get the material structure and include fixed connection at the telescopic link one of elevator rear end face, telescopic link one inner chamber sliding connection has telescopic link two, the equal fixedly connected with in the outer surface lower part of telescopic link and the clamping jaw that reaction structure matches each other, two inner chambers sliding connection of telescopic link have telescopic link three, the three adjacent one side inner chambers of telescopic link rotate and are connected with the stationary dog, three left end face fixedly connected with sampling motor of telescopic link, sampling motor output and stationary dog fixed connection.
Compared with the prior art, the invention provides a preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomers, which has the following beneficial effects:
1. the method can efficiently prepare the CuZnAl ternary alloy catalyst powder with excellent quality, has safer and more reasonable production process, constant and controllable quality, is suitable for batch production, can obviously improve the quality of finished products, and reduces the production cost.
2. The diffusion furnace disclosed by the invention has the advantages that the inner cavity of the device is sealed through the protective structure on the upper end surface of the bottom plate, the inner cavity of the device is kept at the set temperature, the gas flow velocity is uniform during use through the barrier structure, the reactant is uniformly contacted, the powder purity is kept at the qualified line level during preparation of the catalyst, and the mixing production efficiency of the flaky nano CuZnAl ternary alloy catalyst powder is improved
3. According to the invention, through the exhaust structure on the front end face of the sealing door, reaction gas is simultaneously exhausted from the device after being used, so that the gas flow rate in the inner cavity of the device is the same, and when the exhaust structure is closed, the inner cavity of the device forms a relatively sealed environment, the purity of a product during reaction is ensured, and through the damping structure on the upper end face of the bottom plate, the device is damped during use, so that the stability of the device is improved, and the vibration brought by a material taking mechanism during material taking and placing is reduced. Through storage structure, the reaction structure of bottom plate upper end to place raw and other materials when using and guarantee that the raw and other materials reaction is even, improve production efficiency.
4. The invention is also provided with a material taking structure which can realize the automatic taking and placing operation of the materials and the storage plate and prevent the danger of scalding caused by the manual taking and placing of operators. The material taking structure is arranged outside the diffusion furnace, the clamping position of the fixed claw can be automatically adjusted, the use is flexible and free, and the convenience and the safety of the use of the equipment are improved.
Drawings
FIG. 1 is a schematic perspective view of the present invention;
FIG. 2 is a rear perspective view of the present invention;
FIG. 3 is a schematic longitudinal half-section perspective view of the present invention;
fig. 4 is a schematic view of a transverse half-section perspective structure of the present invention.
In the figure: 1-bottom plate, 2-protective structure, 21-protective plate, 22-air inlet, 3-top plate, 4-sealing door, 41-sealing plate, 42-pneumatic telescopic rod, 5-exhaust structure, 51-exhaust frame, 52-sealing grid, 53-exhaust frame, 54-rotating shaft, 55-fan blade, 6-damping structure, 61-sliding rod, 62-spring, 63-sliding block, 64-rotating rod, 65-placing plate, 7-storage structure, 71-supporting rod, 72-placing groove, 73-protective plate, 8-reaction structure, 81-storage plate, 82-air conveying groove, 83-reaction groove, 9-blocking structure, 91-blocking frame, 92-connecting plate, 93-blocking plate, 10-controller, 101-control panel, 102-display screen, 103-control button, 11-heater, 12-rotating rod, 13-driving structure, 131-driving motor, 132-belt pulley, 133-belt, 14-driving structure, 141-gear, 142-gear, 15-lifting structure, 151-152-threaded rod, 151-lifting and 163-lifting block, 163-lifting structure, 162-telescopic rod-lifting structure, and 162-telescopic rod-sampling structure.
Detailed Description
Example 1
The invention relates to a preparation method of CuZnAl ternary alloy catalyst powder for synthesizing an organic silicon monomer, which comprises the following steps:
1) Firstly, putting electrolytic copper, a standard zinc ingot and a standard aluminum ingot into a melting furnace for melting according to the mass part ratio of 10 parts to 4 parts; firstly, adding an aluminum ingot and a zinc ingot into a smelting furnace, covering the aluminum ingot and the zinc ingot with charcoal, and then adding electrolytic copper; when the smelting temperature is 700 ℃, precursor powder is prepared by adopting a water atomization process, and the atomization pressure is not less than 20MPa;
2) Adding 2 parts of pure copper powder into the precursor powder, and uniformly mixing by adopting a mixer to prepare mixed powder of CuZnAl and copper;
3) Sending the mixed powder of CuZnAl and copper into a diffusion furnace for diffusion treatment, wherein the furnace temperature is 650 ℃, and then performing diffusion treatment on the mixed powder for 2 hours under the temperature condition;
4) Crushing the CuZnAl alloy product obtained after diffusion to obtain CuZnAl alloy powder;
5) Screening the crushed CuZnAl alloy powder by using a 150-micron screen, and taking undersize;
6) And adding the crushed powder into a high-energy ball mill filled with nitrogen, and performing ball milling to obtain flaky nano CuZnAl ternary alloy catalyst powder.
Further, in the step 1), the particle size of the atomized powder is less than 45um.
Further, in the step 2), the pure copper powder is atomized copper powder, and the purity is not lower than 99.6%.
Further, the pulverizer in the step 4) is a universal pulverizer. The high-energy ball mill in the step 5) is a dry ball mill; the rotating speed is not lower than 300r/min, and the nitrogen purity is not lower than 99.999 percent
As shown in fig. 1-4, the diffusion furnace in step 3) includes a bottom plate 1, a protection structure 2 is fixedly connected to an upper end face of the bottom plate 1, a top plate 3 is fixedly connected to an upper end face of the protection structure 2, sealing doors 4 are symmetrically hinged to front end faces of the protection structure 2, an exhaust structure 5 is fixedly connected to middle portions of front end faces of the two sealing doors 4, a damping structure 6 is arranged at the middle portion of the upper end face of the bottom plate 1, a storage structure 7 is fixedly connected to an upper end face of the damping structure 6, a reaction structure 8 is uniformly slidably clamped in an inner cavity of the storage structure 7, a blocking structure 9 is fixedly connected to rear ends of the inner cavity of the protection structure 2, the blocking structures 9 are fixedly connected to four corners of the lower end face of the bottom plate 1, a control panel 10 is fixedly connected to the left side of the upper portion of the rear end face of the protection structure 2, a heater 11 is fixedly connected to the middle portion of the lower end face of the top plate 3, a placement frame 12 is fixedly connected to the upper end face of the placement frame 12, a driving structure 13 is fixedly connected to the middle portion of the upper end face of the placement frame 12, a transmission structure 14 is fixedly connected to the upper end face of the transmission structure 14 is fixedly connected to a lifting structure 15, and a material taking structure 16 is symmetrically fixedly connected to the rear end face of the lifting structure 15.
Exhaust structure 5 includes fixed connection at the exhaust frame 51 at terminal surface middle part before sealing door 4, and the even rotation in exhaust frame 51 inner chamber left side is connected with sealed grid 52, and exhaust frame 51 inner chamber symmetry fixedly connected with exhaust frame 53, exhaust frame 53 inner chamber rotate and connect axis of rotation 54, axis of rotation 54 inner chamber fixedly connected with micro motor, the even fixedly connected with flabellum 55 in axis of rotation 54 surface, micro motor output and flabellum 55 fixed connection.
Shock-absorbing structure 6 includes the slide bar 61 of symmetry fixed connection in the inner chamber lower part of guard plate 21, slide bar 61 surface activity has cup jointed spring 62, slide bar 61 surface symmetry sliding connection has slider 63, the spring 62 both ends respectively with two slider 63 fixed connection, 6 up ends of slider rotate the one end that is connected with dwang 64 through the rotating turret, board 65 is placed through another rotating turret fixedly connected with to the dwang 64 other end, place board 65 up end fixedly connected with storage structure 7, place the terminal surface middle part fixedly connected with telescopic link under the board 65, terminal surface and bottom plate 1 fixed connection under the telescopic link.
Storage structure 7 includes fixed connection at the bracing piece 71 of placing board 63 up end four corners, the even fixedly connected with standing groove 72 of bracing piece 71 adjacent one side inner chamber, bracing piece 71 up end fixedly connected with guard plate 73, reaction structure 8 is connected to standing groove 72 inner chamber slip joint.
The control panel 10 comprises a control panel 101 fixedly connected to the upper portion of the left side of the rear end face of the protection plate 21, a display 102 is fixedly connected to the upper portion of the front end face of the control panel 101, and a control button 103 is uniformly and fixedly connected to the lower portion of the front end face of the control panel 101.
The heater 11 circuit is connected with the protection plate 21 and electrically connected with the control panel 101 of the controller 10, the micro motor in the inner cavity of the exhaust structure 5 is connected with the micro motor, and the protection plate 21 is electrically connected with the control panel 101 in the controller 10.
One side of the inner cavity side of the protection plate 21 is fixedly connected with a temperature detection structure, and the temperature detection structure is electrically connected with the control panel 101.
The driving structure 13 includes a driving motor 131 fixedly connected to the middle portion of the upper end face of the placing frame 12, an output end of the driving motor 131 is fixedly connected to a belt pulley 132, an outer surface of the belt pulley 132 is in transmission connection with one end of a belt 133, one end of the belt 133 is in transmission connection with another belt pulley 132, and the other belt pulley 132 is fixedly connected to the driving structure 14.
The material taking structure 16 comprises a first telescopic rod 161 fixedly connected to the rear end face of the lifting block 152, a second telescopic rod 162 is connected to the inner cavity of the first telescopic rod 161 in a sliding mode, clamping jaws matched with the reaction structure 8 are fixedly connected to the lower portion of the outer surface of the second telescopic rod 162, a third telescopic rod 164 is connected to the inner cavity of the second telescopic rod 162 in a sliding mode, a fixing claw 164 is rotatably connected to the inner cavity of one side, adjacent to the third telescopic rod 164, a sampling motor 165 is fixedly connected to the left end face of the third telescopic rod 164, and the output end of the sampling motor 165 is fixedly connected with the fixing claw 164.
The working principle and the using process of the invention are as follows:
in operation, the mixed powder of CuZnAl and copper is placed in the inner cavity of the reaction tank 83, the sealing door 4 is pulled at the moment, the storage plate 81 is sequentially placed in the inner cavity of the placing tank 72, the sealing door 4 is closed at the moment, the inner cavity of the device forms a relatively sealed environment, the output end of the air intake machine is connected with the air inlet 22, the airflow velocity is reduced due to the blocking plate 93, so that the gas is uniformly distributed, the production efficiency is increased during the production of reactants, the mixed powder of CuZnAl and copper at the upper part is mixed with the gas, the production efficiency is improved, when the device vibrates, the rotating rod 64 rotates, so that the sliding block 63 relatively slides, the spring 62 stretches, the placing plate 65 is lifted to the height, the reaction raw material in the inner cavity of the reaction tank 83 is damped, the raw material is prevented from being poured during the vibration of the device, the production cost is increased, and the raw material inclines on one side, the reaction rate is different during production, the yield of single crystal production is influenced, the single crystal production is further controlled by the controller 10 when the single crystal production is used, the reaction device is kept at about 650 ℃ of reaction setting within a certain time, meanwhile, because the temperature detection structure is arranged on the side part of the inner cavity of the protective structure 2, the temperature in the furnace is conveniently detected in real time when the single crystal production device is used, the reaction is kept under a proper condition for a long time, the reaction is always in an optimal stage, when the reaction is finished, the driving motor 131 is started, the belt pulley 132 is rotated, the belt 133 is rotated, the rotating rod 141 is rotated, the gear 142 is rotated, the threaded rod 151 is rotated, the lifting block 152 is further lifted, the first telescopic rod 161 is started at the moment, the second telescopic rod 162 is extended, and the clamping jaw is clamped with the front end face of the storage plate 81, further make three 163 of telescopic link flexible to make sample motor 165 output rotate, so the stationary dog 164 takes place to rotate, and then makes stationary dog 164 and memory board 81 back block, thereby accesses reaction structure 8, when avoiding manual storage, personnel receive the high temperature injury.
Example 2
The invention provides a preparation method of CuZnAl ternary alloy catalyst powder for synthesizing an organic silicon monomer, which comprises the following steps:
(1) Firstly, putting electrolytic copper, a standard zinc ingot and a standard aluminum ingot into a melting furnace for melting according to the mass part ratio of 10 parts to 5 parts; firstly, adding an aluminum ingot and a zinc ingot into a smelting furnace, covering the aluminum ingot and the zinc ingot with charcoal, and then adding electrolytic copper; when the smelting temperature is 700 ℃, preparing precursor powder by adopting a water atomization process, wherein the atomization pressure is not less than 20MPa;
(2) Adding 3 parts of pure copper powder into the precursor powder, and uniformly mixing by adopting a mixer to prepare mixed powder of CuZnAl and copper;
(3) Sending the mixed powder of CuZnAl and copper into a diffusion furnace for diffusion treatment, wherein the furnace temperature is 650 ℃, and then performing diffusion treatment on the mixed powder for 3 hours under the temperature condition;
(4) Crushing the CuZnAl alloy product obtained after diffusion to obtain CuZnAl alloy powder;
(5) Screening the crushed CuZnAl alloy powder by using a 150-micron screen, and taking undersize;
(6) And adding the crushed powder into a high-energy ball mill filled with nitrogen, and carrying out ball milling to obtain the flaky nano CuZnAl ternary alloy catalyst powder.
The rest of this embodiment is the same as embodiment 1, and will not be described again.
Example 3
The invention provides a preparation method of CuZnAl ternary alloy catalyst powder for synthesizing an organic silicon monomer, which comprises the following steps:
(1) Firstly, putting electrolytic copper, a standard zinc ingot and a standard aluminum ingot into a melting furnace for melting according to the mass part ratio of 10 parts to 6 parts; firstly, adding an aluminum ingot and a zinc ingot into a smelting furnace, covering the aluminum ingot and the zinc ingot with charcoal, and then adding electrolytic copper; when the smelting temperature is 700 ℃, preparing precursor powder by adopting a water atomization process, wherein the atomization pressure is not less than 20MPa;
(2) Adding 5 parts of pure copper powder into the precursor powder, and uniformly mixing by adopting a mixer to prepare mixed powder of CuZnAl and copper;
(3) Sending the mixed powder of CuZnAl and copper into a diffusion furnace for diffusion treatment, wherein the furnace temperature is 650 ℃, and then performing diffusion treatment on the mixed powder for 4 hours under the temperature condition;
(4) Crushing the CuZnAl alloy product obtained after diffusion to obtain CuZnAl alloy powder;
(5) Screening the crushed CuZnAl alloy powder by using a 150-micron screen, and taking undersize;
(6) And adding the crushed powder into a high-energy ball mill filled with nitrogen, and carrying out ball milling to obtain the flaky nano CuZnAl ternary alloy catalyst powder.
The rest of this embodiment is the same as embodiment 1, and will not be described again.
It is to be understood that the present invention has been described with reference to certain embodiments and that various changes in form and details may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. A preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomers is characterized by comprising the following steps:
1) Firstly, putting electrolytic copper, a standard zinc ingot and a standard aluminum ingot into a melting furnace for melting according to the mass part ratio of 10 parts to 4-6 parts; firstly, adding an aluminum ingot and a zinc ingot into a smelting furnace, covering the aluminum ingot and the zinc ingot with charcoal, and then adding electrolytic copper; when the smelting temperature is 700 ℃, precursor powder is prepared by adopting a water atomization process, and the atomization pressure is not less than 20MPa;
2) Adding 2-5 parts of pure copper powder into the precursor powder, and uniformly mixing by adopting a mixer to prepare mixed powder of CuZnAl and copper;
3) Sending the mixed powder of CuZnAl and copper into a diffusion furnace for diffusion treatment, wherein the furnace temperature is 650 ℃, and then performing diffusion treatment on the mixed powder for 2 to 4 hours under the temperature condition;
4) Crushing the CuZnAl alloy product obtained after diffusion to obtain CuZnAl alloy powder;
5) Screening the crushed CuZnAl alloy powder by using a 150-micron screen, and taking undersize;
6) And adding the crushed powder into a high-energy ball mill filled with nitrogen, and carrying out ball milling to obtain the flaky nano CuZnAl ternary alloy catalyst powder.
2. The method for preparing CuZnAl ternary alloy catalyst powder for synthesizing organosilicon monomers according to claim 1, wherein the particle size of the atomized powder in the step 1) is less than 45um.
3. The method for preparing CuZnAl ternary alloy catalyst powder for organosilicon monomer synthesis according to claim 1, wherein in step 2), the pure copper powder is atomized copper powder, and the purity is not less than 99.6%.
4. The method for preparing CuZnAl ternary alloy catalyst powder for organosilicon monomer synthesis according to claim 1, wherein the pulverizer in step 4) is a universal pulverizer, the high-energy ball mill in step 5) is a dry ball mill, the rotation speed is not lower than 300r/min, and the nitrogen purity is not lower than 99.999%.
5. The preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organosilicon monomers, according to claim 1, characterized in that, in the step (3), the diffusion furnace comprises a bottom plate (1), a protective structure (2) is fixedly connected to the upper end face of the bottom plate (1), a top plate (3) is fixedly connected to the upper end face of the protective structure (2), a sealing door (4) is symmetrically hinged to the front end face of the protective structure (2), two exhaust structures (5) are fixedly connected to the middle of the front end face of the sealing door (4), a damping structure (6) is arranged at the middle of the upper end face of the bottom plate (1), a storage structure (7) is fixedly connected to the upper end face of the damping structure (6), a reaction structure (8) is uniformly clamped in a sliding manner in an inner cavity of the storage structure (7), a blocking structure (9) is fixedly connected to the rear end face of the inner cavity of the protective structure (2), blocking structures (9) are fixedly connected to four corners of the lower end face of the bottom plate (1), a control panel (10) is fixedly connected to the left side of the upper portion of the rear end face of the protective structure (2), a heater (11) is fixedly connected to the lower end face of the top plate (3), a driving structure (14) is fixedly connected to the upper end face of a driving structure (14), the rear end face of the lifting structure (15) is symmetrically and fixedly connected with a material taking structure (16).
6. The preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organosilicon monomers according to claim 5, characterized in that the protective structure (2) comprises a protective plate (21) fixedly connected to the upper end surface of the bottom plate (1), the middle part of the rear end surface of the protective plate (21) is fixedly connected with an air inlet (22), the shock absorption structure (6) is fixedly connected to the middle part of the lower end surface of the inner cavity of the protective plate (21), the sealing door (4) comprises sealing plates (42) hinged to both sides of the front end surface of the protective plate (21), the upper end surfaces of the sealing plates (42) are rotatably connected with one end of a pneumatic telescopic rod (41), and the other end of the pneumatic telescopic rod (41) is rotatably connected with the upper end surface of the top plate (3);
exhaust structure (5) are including exhaust frame (51) of fixed connection at the front end face middle part of sealing door (4), the even rotation in exhaust frame (51) inner chamber left side is connected with sealed grid (52), exhaust frame (51) inner chamber symmetry fixedly connected with exhaust frame (53), rotation axis (54) is connected in exhaust frame (53) inner chamber rotation, rotation axis (54) inner chamber fixedly connected with micro motor, the even fixedly connected with flabellum (55) of rotation axis (54) surface, micro motor output and flabellum (55) fixed connection.
7. The preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomer according to claim 6, wherein the shock-absorbing structure (6) comprises a slide bar (61) symmetrically and fixedly connected to the lower part of the inner cavity of the protection plate (21), a spring (62) is movably sleeved on the outer surface of the slide bar (61), a slide block (63) is symmetrically and slidably connected to the outer surface of the slide bar (61), two ends of the spring (62) are respectively and fixedly connected to the two slide blocks (63), the upper end surface of the slide block (6) is rotatably connected to one end of a rotating rod (64) through a rotating frame, the other end of the rotating rod (64) is fixedly connected to a placing plate (65) through another rotating frame, the upper end surface of the placing plate (65) is fixedly connected to a storage structure (7), the middle part of the lower end surface of the placing plate (65) is fixedly connected to a telescopic rod, and the lower end surface of the telescopic rod is fixedly connected to the bottom plate (1).
8. The preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organosilicon monomers, according to claim 7, characterized in that the storage structure (7) comprises support bars (71) fixedly connected at four corners of the upper end surface of the placing plate (63), wherein the inner cavities of the adjacent sides of the support bars (71) are uniformly and fixedly connected with placing grooves (72), the upper end surface of the support bars (71) is fixedly connected with a protection plate (73), and the inner cavities of the placing grooves (72) are slidably clamped with the reaction structures (8).
9. The preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organosilicon monomers according to claim 8, wherein the reaction structure (8) comprises a storage plate (81) which is slidably clamped in an inner cavity of the placement groove (72), the front end surface of the storage plate (81) is uniformly and fixedly connected with a gas transmission groove (82) in a penetrating manner, the upper end surface of the storage plate (81) is uniformly and fixedly connected with a reaction groove (83), the gas transmission groove (82) is connected with the reaction groove (83) in a penetrating manner, the blocking structure (9) comprises a blocking frame (91) which is fixedly connected at the rear part of the inner cavity of the protection plate (21), the upper end surface of the blocking frame (91) is fixedly connected with the top plate (3), the rear end surface of the inner cavity of the blocking frame (91) is fixedly connected with a connecting plate (92), the rear end surface of the connecting plate (92) is fixedly connected with a blocking plate (93), and the blocking plate (93) is matched with the gas inlet (22).
10. The preparation method of CuZnAl ternary alloy catalyst powder for synthesizing organic silicon monomer according to claim 9, wherein the driving structure (13) comprises a driving motor (131) fixedly connected to the middle part of the upper end surface of the placing frame (12), the output end of the driving motor (131) is fixedly connected with a belt pulley (132), the outer surface of the belt pulley (132) is in transmission connection with one end of a belt (133), one end of the belt (133) is in transmission connection with another belt pulley (132), and the other belt pulley (132) is fixedly connected with the transmission structure (14);
the transmission structure (14) comprises gears (142) which are symmetrically and rotatably connected to the front part of the upper end face of the placing frame (12), rotating rods (141) are arranged at the rear parts of the gears (142) and rotatably connected with the placing plate (12), threads in opposite directions are arranged on two sides of the outer surface of each rotating rod (141), the threads on the outer surface of each rotating rod (141) are meshed with the gears (142), the belt pulley (132) is fixedly connected to the middle part of the outer surface of each rotating rod (141), and the lifting structure (15) is fixedly connected to the upper end face of each gear (142);
the lifting structure (15) comprises a threaded rod (151) fixedly connected to the upper end face of the gear (142), the outer surface of the threaded rod (151) is in threaded connection with a lifting block (152), the middle part of one adjacent side of the lifting block (152) is fixedly connected with a limiting rod, and the rear end face of the lifting block (152) is fixedly connected with a material taking structure (16);
get material structure (16) and include telescopic link one (161) of fixed connection at elevator block (152) rear end face, telescopic link one (161) inner chamber sliding connection has telescopic link two (162), the equal fixedly connected with in telescopic link two (162) surface lower part and the clamping jaw that reaction structure 8 matches each other, telescopic link two (162) inner chamber sliding connection has telescopic link three (164), the adjacent one side inner chamber of telescopic link three (164) rotates and is connected with stationary dog (164), three (164) left end face fixedly connected with sampling motor (165) of telescopic link, sampling motor (165) output and stationary dog (164) fixed connection.
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