CN114904585A - Preparation method of palladium-carbon catalyst for Suzuki coupling reaction - Google Patents
Preparation method of palladium-carbon catalyst for Suzuki coupling reaction Download PDFInfo
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- CN114904585A CN114904585A CN202210549630.9A CN202210549630A CN114904585A CN 114904585 A CN114904585 A CN 114904585A CN 202210549630 A CN202210549630 A CN 202210549630A CN 114904585 A CN114904585 A CN 114904585A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/24—Phosphines, i.e. phosphorus bonded to only carbon atoms, or to both carbon and hydrogen atoms, including e.g. sp2-hybridised phosphorus compounds such as phosphabenzene, phosphole or anionic phospholide ligands
- B01J31/2404—Cyclic ligands, including e.g. non-condensed polycyclic ligands, the phosphine-P atom being a ring member or a substituent on the ring
- B01J31/2409—Cyclic ligands, including e.g. non-condensed polycyclic ligands, the phosphine-P atom being a ring member or a substituent on the ring with more than one complexing phosphine-P atom
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
- F26B3/04—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour circulating over or surrounding the materials or objects to be dried
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/40—Substitution reactions at carbon centres, e.g. C-C or C-X, i.e. carbon-hetero atom, cross-coupling, C-H activation or ring-opening reactions
- B01J2231/42—Catalytic cross-coupling, i.e. connection of previously not connected C-atoms or C- and X-atoms without rearrangement
- B01J2231/4205—C-C cross-coupling, e.g. metal catalyzed or Friedel-Crafts type
- B01J2231/4211—Suzuki-type, i.e. RY + R'B(OR)2, in which R, R' are optionally substituted alkyl, alkenyl, aryl, acyl and Y is the leaving group
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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
- Y02P20/584—Recycling of catalysts
Abstract
The application relates to a preparation method of a palladium-carbon catalyst for Suzuki coupling reaction, which comprises the following steps: s1: boiling and activating coconut shell activated carbon by using 5% -10% dilute nitric acid, then washing the activated carbon to be neutral by using deionized water, drying and smashing the activated carbon by shaking; s2: metering the coconut shell activated carbon treated in the step S1, adding the coconut shell activated carbon into an alcohol solution containing a phosphorus ligand for impregnation, wherein the impregnation temperature is controlled to be 50-60 ℃, and then removing the solvent to obtain triphenylphosphine-loaded activated carbon; s3: pulping the triphenylphosphine-loaded active carbon and tetraamminepalladium bicarbonate by using water, ethanol or ethylene glycol; s4: controlling the temperature at 80-100 ℃, and introducing hydrogen to reduce for 3-4h to obtain the palladium-carbon catalyst. This application has and carries out the shattering and improve the coconut husk active carbon and carry out the impregnation effect in follow-up step to improving to the coconut husk active carbon.
Description
Technical Field
The application relates to the field of dryers, in particular to a preparation method of a palladium-carbon catalyst for Suzuki coupling reaction.
Background
The palladium carbon catalyst is a common hydrogenation catalyst and a coupling catalyst, and is widely applied to Suzuki coupling reaction.
For example, chinese patent application publication No. CN106824267A discloses a palladium-carbon catalyst for Suzuki coupling reaction and a preparation method thereof, which specifically includes the following process steps:
s1: boiling and activating coconut shell activated carbon by using 5% -10% dilute nitric acid, washing the activated carbon to be neutral by using deionized water, and drying the activated carbon;
s2: metering the coconut shell activated carbon treated in the step S1, adding the coconut shell activated carbon into an alcoholic solution containing a phosphorus ligand for impregnation, wherein the impregnation temperature is controlled to be 50-60 ℃, and then removing the solvent to obtain triphenylphosphine-loaded activated carbon;
s3: pulping the triphenylphosphine-loaded active carbon and tetraamminepalladium bicarbonate by using water, ethanol or ethylene glycol;
s4: controlling the temperature at 80-100 ℃, and introducing hydrogen to reduce for 3-4h to obtain the palladium-carbon catalyst.
With respect to the related art among the above, the inventors consider that the following drawbacks exist: when the coconut shell activated carbon is dried, a plurality of coconut shell activated carbons may be adhered together due to the existence of water, and the subsequent impregnation efficiency of the coconut shell activated carbon is affected by the adhesion condition after the drying.
Disclosure of Invention
In order to reduce the occurrence of the condition that a plurality of coconut shell activated carbons are adhered together during drying and improve the impregnation efficiency of the subsequent coconut shell activated carbons, the application provides a preparation method of a palladium-carbon catalyst for Suzuki coupling reaction.
The preparation method of the palladium-carbon catalyst for the Suzuki coupling reaction adopts the following technical scheme:
a preparation method of a palladium-carbon catalyst for Suzuki coupling reaction is characterized by comprising the following steps:
s1: boiling and activating coconut shell activated carbon by using 5% -10% dilute nitric acid, then washing the activated carbon to be neutral by using deionized water, drying and smashing the activated carbon by shaking;
s2: metering the coconut shell activated carbon treated in the step S1, adding the coconut shell activated carbon into an alcoholic solution containing a phosphorus ligand for impregnation, wherein the impregnation temperature is controlled to be 50-60 ℃, and then removing the solvent to obtain triphenylphosphine-loaded activated carbon;
s3: pulping the triphenylphosphine-loaded active carbon and tetraamminepalladium bicarbonate by using water, ethanol or ethylene glycol;
s4: controlling the temperature at 80-100 ℃, and introducing hydrogen to reduce for 3-4h to obtain the palladium-carbon catalyst.
Through adopting above-mentioned technical scheme, shake garrulous to the coconut husk active carbon when will drying, reduce the adhesion of coconut husk active carbon when drying together, lead to the drying effect variation to the coconut husk active carbon when drying to make the condition emergence that the coconut husk active carbon impregnation efficiency in the follow-up step offsets.
Optionally, the device for drying and shattering in S1 includes a frame, a driving assembly for driving a plurality of raw materials to move is disposed on the frame, the driving assembly includes two rotating rollers, a driving motor for driving the rotating rollers to rotate, and a mesh belt for blocking the raw materials, both the two rotating rollers are rotatably connected to the frame, the mesh belt is sleeved on the two rotating rollers, an air blowing assembly for intermittently blowing hot air to the mesh belt is disposed under the mesh belt, and the air blowing assembly includes an air blowing pipe and an air blowing member for intermittently blowing air to the air blowing pipe; the air blowing pipe and the air blowing piece are arranged on the rack.
Through adopting above-mentioned technical scheme, during the use, the piece of blowing blows off steam to the gas blow pipe indirectness for steam in the gas blow pipe dries and blows off to a certain extent the raw materials on the guipure, and the reduction raw materials takes place because the existence of water bonds the condition together when drying to the raw materials, improves the drying efficiency to the raw materials.
Optionally, the air blowing piece comprises an air bag, a first air blower for continuously inflating the air bag, a heating structure for heating air blown out by the first air blower, and an opening and closing structure for intermittently opening and closing the air bag; the air blowing pipe is communicated with the air bag, and the opening and closing structure is positioned in the air blowing pipe.
Through adopting above-mentioned technical scheme, after gathering up pressure through the gasbag, open and close the structure and open the gasbag for the gas pressure who blows off is bigger, makes the raw materials more can be blown away, further improves the drying efficiency to the raw materials.
Optionally, a sponge layer for storing and absorbing water for the raw materials is arranged on the machine frame, the sponge layer is positioned right above the air blowing pipe, and a plurality of storage holes for storing and absorbing water for the raw materials are formed in one end face, close to the mesh belt, of the sponge layer; and a water absorption layer is arranged at one end of the sponge layer, which is far away from the mesh belt.
By adopting the technical scheme, the blowing assembly blows the raw materials on the mesh belt, the raw materials originally positioned in the storage holes are blown off, one part of the blown raw materials enter the storage holes, the other part of the blown raw materials are abutted against the sponge layer, the sponge layer absorbs the raw materials, the blowing assembly enables the raw materials originally positioned in the storage holes to fall off, and the raw materials on the mesh belt enter the storage holes, so that the structure is simple; after long-time use, the intraformational water of sponge will increase, and unnecessary water in the sponge will enter into the hydroscopic layer, increases the live time on sponge layer.
Optionally, the opening and closing structure comprises a connecting rod, a mounting block, a chock block and a plurality of extrusion rods; the installation piece sets up in blowing pipe, the one end that the gasbag was kept away from to the installation piece has seted up the bell mouth, the chock slides and connects in the bell mouth and be used for blockking up the bell mouth, connecting rod one end sets up on the chock, and is a plurality of the stripper bar set up in the one end that the chock was kept away from to the connecting rod, it is a plurality of the stripper bar is used for the extrusion the sponge layer.
By adopting the technical scheme, when the inflatable air bag is used, the first air blower is continuously inflated to blow the air bag large, so that the pressure in the air bag is increased, then the plug block vertically moves upwards under the action of gas in the air bag, so that the air bag is opened, and then the gas is blown to the mesh belt; when the chock vertically moves upwards, the connecting rod and the plurality of extrusion rods on the connecting rod move along the direction close to the sponge layer, so that the plurality of extrusion rods extrude the sponge layer, gas in the blowing pipe blows out and also extrudes the sponge layer to a certain extent, on one hand, moisture in the sponge layer is extruded into the water absorption layer, on the other hand, raw materials originally positioned in the storage hole fall onto the mesh belt, and when the raw materials originally positioned in the storage hole fall onto the mesh belt, the raw materials are collided with blown raw materials, so that the moisture on the raw materials is more easily thrown out and crashed; realize drying the raw materials on the guipure and blowing off, realize extrudeing the sponge layer for the intraformational water of sponge is extruded to the in situ that absorbs water, improves the effect that absorbs water of sponge layer to the raw materials.
Optionally, an air drying assembly for blowing away most of water in the raw material is arranged on the rack, the air drying assembly includes two holding pipes, a hollow ring pipe and an air supply member for continuously supplying air to the hollow ring pipe, the hollow ring pipe is located between the two holding pipes, the holding pipes are arranged on the hollow ring pipe, a plurality of air outlets are formed in the inner wall of the hollow ring pipe, and the mesh belt penetrates through the two holding pipes and the hollow ring pipe.
Through adopting above-mentioned technical scheme, during the use, air feed spare carries out the air feed to in to the cavity ring, and gas blows to the raw materials of guipure through the air outlet on for most water on the raw materials on the guipure is blown away by the wind that the air outlet blew off, keeps the pipe to keep the raw materials on the guipure, further improves the efficiency that the gas blow pipe dried to the raw materials on the guipure.
Optionally, a recovery assembly for utilizing redundant hot air discharged from the air bag is arranged on the frame, and the recovery assembly comprises a recovery box body and a recycling pipe; the sponge layer, the water absorbing layer and the air blowing pipe are located in the recovery box body, and a material passing through hole for the mesh belt to penetrate through is formed in the recovery box body.
Through adopting above-mentioned technical scheme, during the use, when the gas blow pipe blows to in the recovery box, partial steam in the recovery box enters into to the cavity ring pipe through the retrieval and utilization pipe in to blow to the guipure through the air outlet on the cavity ring pipe, realize carrying out recycle to the partial heat in the recovery box, improve the utilization to the energy, green.
Optionally, a blocking assembly for blocking the material passing through hole when the air blowing pipe blows air is arranged in the recovery box body, and the blocking assembly comprises a blocking door for blocking the material passing through hole and a driving structure for driving the blocking door to move; the stop gate is connected on the recovery box body inside wall in a sliding manner.
Through adopting above-mentioned technical scheme, drive structure drives when the gas blow pipe blows and blocks the door and remove and make and block the door and block the material through-hole, makes the steam in the recovery box enter into the air outlet department on the cavity ring canal through the retrieval and utilization pipe, realizes carrying out cyclic utilization to unnecessary steam in the recovery box, further improves the stoving effect of air outlet to the raw materials.
Optionally, it slides along the connecting rod glide direction and connects on retrieving the box inside wall to block the door, the drive structure includes reversing gear, driven rack and initiative rack, driven rack set up in block on the door, initiative rack sets up on the connecting rod, the reversing gear is located between driven rack and the initiative rack, the reversing gear rotates and connects on retrieving the inside wall of box, the reversing gear all meshes with driven rack and initiative rack mutually.
Through adopting above-mentioned technical scheme, when the vertical rebound of chock, the initiative rack on connecting rod and the connecting rod is also along with the vertical rebound of chock, the initiative rack passes through the reversing gear and drives driven rack along vertical rebound, make and block the door and block the material through-hole, it overflows to reduce the heat in the recovery box through the material through-hole, when the realization is blown at the gas blow pipe, the realization blocks the door and blocks the material through-hole, when blocking the door and block the material through-hole, block that the door carries out the subregion with the raw materials on the guipure, the realization is to carrying out initial segregation and further crushing to the raw materials on the guipure, make things convenient for subsequent drying and dissolve.
Optionally, a maintaining assembly for maintaining a distance between the blocking door and the rack is arranged between the blocking door and the rack, and the maintaining assembly comprises a maintaining spring, an installation rod and a nut; the installation rod length direction is parallel with the sliding direction of the stop gate, the stop gate is connected on the installation rod in a sliding manner, the nut is connected on the installation rod in a threaded manner, the maintaining spring is sleeved on the installation rod, the maintaining spring is located between the nut and the stop gate, one end of the maintaining spring is abutted to the nut, and the other end of the maintaining spring is arranged on the stop gate.
Through adopting above-mentioned technical scheme, during the use, operating personnel accessible rotates adjusting nut and realizes the regulation to maintaining spring force, realizes the regulation to the pressure of chock, bell mouth, realizes the regulation to the gas pressure size of following the gas pocket.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the raw materials on the mesh belt are blown away and dried through the blowing assembly, so that the drying efficiency of the raw materials is further improved;
2. the air bag is opened or closed and the sponge layer is extruded and pressurized by the blowing piece and the opening and closing structure;
3. through opening and close the structure and block the subassembly, realize opening or closing the stop gate in the in-process that extrudees the pressurized-water to the sponge layer, reduce thermal loss.
Drawings
Fig. 1 is a schematic structural diagram of a specific embodiment of the present application.
Fig. 2 is a schematic diagram of the air stem assembly of fig. 1.
Fig. 3 is a cross-sectional view of fig. 1 showing the structure within the recovery tank.
FIG. 4 is a cross-sectional view of FIG. 3, showing the construction of the blowing assembly, the sponge layer, and the water absorbent layer.
Fig. 5 is an enlarged view at a in fig. 4 for showing the structure of the chock and the mounting block.
Fig. 6 is a structure of the barrier gate and the driving structure of fig. 3.
Reference numerals: 1. a frame; 11. a drive assembly; 111. a drive motor; 112. a mesh belt; 2. air-drying the assembly; 21. a holding tube; 22. a hollow collar; 23. a gas supply member; 231. a gas supply pipe; 232. a second blower; 24. an air outlet; 3. a recovery assembly; 31. a recovery box body; 32. a recycling pipe; 33. a material through hole; 4. a sponge layer; 41. a polyacrylamide layer; 42. a storage hole; 5. a blowing assembly; 51. an air blowing pipe; 52. an air blowing member; 521. an air bag; 522. an inflation tube; 523. a first blower; 524. a heating structure; 5241. heating the box body; 5242. heating resistance wires; 525. an opening and closing structure; 5251. a connecting rod; 5252. installing a frame; 5253. mounting blocks; 5254. a chock block; 5255. an extrusion stem; 526. a tapered hole; 6. a blocking component; 61. a U-shaped frame; 62. a blocking door; 63. a drive structure; 631. a reversing gear; 632. fixing the rod; 633. a driven rack; 634. a driving rack; 7. a maintenance assembly; 71. a retaining spring; 72. a fixing plate; 73. mounting a rod; 74. and a nut.
Detailed Description
The present application is described in further detail below with reference to figures 1-6.
The embodiment of the application discloses a preparation method of a palladium-carbon catalyst for Suzuki coupling reaction. Referring to fig. 1, a method for preparing a palladium-carbon catalyst for Suzuki coupling reaction includes the following steps:
s1: boiling and activating coconut shell activated carbon by using 5% -10% dilute nitric acid, then washing the activated carbon to be neutral by using deionized water, drying and smashing the activated carbon by shaking;
s2: metering the coconut shell activated carbon treated in the step S1, adding the coconut shell activated carbon into an alcoholic solution containing a phosphorus ligand for impregnation, wherein the impregnation temperature is controlled to be 50-60 ℃, and then removing the solvent to obtain triphenylphosphine-loaded activated carbon;
s3: pulping the triphenylphosphine-loaded active carbon and tetraamminepalladium bicarbonate by using water, ethanol or ethylene glycol;
s4: controlling the temperature at 80-100 ℃, and introducing hydrogen to reduce for 3-4h to obtain the palladium-carbon catalyst.
The device that the stoving in S1 was smashed with shaking includes frame 1, is provided with the drive assembly 11 that is used for driving the removal of coconut husk active carbon in frame 1, has set gradually along coconut husk active carbon direction of motion in frame 1 and has air-dried subassembly 2 and retrieve subassembly 3, is provided with the subassembly 5 of blowing that is used for carrying out the indirectness to the coconut husk active carbon on the drive assembly 11 in retrieving the subassembly 3.
Referring to fig. 1, the driving assembly 11 includes two rotating rollers, a driving motor 111 for driving the rotating rollers to rotate, and a mesh belt 112 for blocking the coconut shell activated carbon; two live rollers rotate and connect in frame 1, and two live rollers distribute along frame 1 length direction, and driving motor 111 fixed connection is in frame 1, and driving motor 111's output shaft and one of them live roller are coaxial fixed connection, and guipure 112 cover is located on two live rollers.
Referring to fig. 1 and 2, the seasoning assembly 2 includes two holding tubes 21, a hollow collar 22, and a gas supply 23 for continuously supplying gas into the hollow collar 22; the hollow ring pipe 22 is positioned between the two holding pipes 21 and coaxially arranged, the holding pipes 21 are fixedly connected to the hollow ring pipe 22, a plurality of air outlets 24 are formed in the inner side wall of the hollow ring pipe 22, the air outlets 24 are uniformly distributed along the axis of the hollow ring pipe 22, and the holding pipes 21 and the hollow ring pipe 22 are both sleeved on the mesh belt 112; the air supply unit 23 includes an air supply pipe 231 and a second blower 232, one end of the air supply pipe 231 is communicated with the outer side wall of the hollow collar 22, and the other end of the air supply pipe 231 is communicated with the second blower 232.
Referring to fig. 1 and 3, the recycling assembly 3 includes a recycling box 31 and a recycling pipe 32, two material through holes 33 distributed along the transportation direction of the coconut shell activated carbon are formed in the recycling box 31, the mesh belt 112 penetrates through the two material through holes 33, one end of the recycling pipe 32 is communicated with the lower end face of the recycling box 31, and the other end of the recycling pipe 32 is communicated with the side wall of the air supply pipe 231.
Referring to fig. 3 and 4, a sponge layer 4 is fixedly connected in the recovery box 31, the sponge layer 4 is positioned right above the mesh belt 112, the upper end surface of the sponge layer 4 is abutted with a water absorption layer, the water absorption layer comprises a polyacrylamide layer 41, and the water absorption layer is fixedly connected on the inner side wall of the recovery box 31; the lower end surface of the sponge layer 4 is provided with a plurality of storage holes 42 for storing coconut shell activated carbon.
Referring to fig. 3 and 4, the blowing assembly 5 includes a blowing pipe 51, a blowing member 52 for intermittently blowing air into the blowing pipe 51; the blowing part 52 comprises an air bag 521, an inflation pipe 522, a first blower 523 for continuously inflating the air bag 521, a heating structure 524 for heating wind blown out by the first blower 523, and an opening and closing structure 525 for intermittently opening and closing the air bag 521; air blowing pipe 51 is vertically arranged, one end of air blowing pipe 51 is fixedly connected to the inner bottom wall of recovery box 31, air blowing pipe 51 penetrates through recovery box 31, air bag 521 is fixedly connected to one end of air blowing pipe 51 penetrating out of recovery box 31, air bag 521 is communicated with air blowing pipe 51, one end of air filling pipe 522 is communicated with air bag 521, and the other end of air filling pipe 522 is communicated with air outlet 24 of first air blower 523.
Referring to fig. 3 and 4, the heating structure 524 includes a heating box 5241 and a heating resistance wire 5242; the heating box 5241 is fixedly connected to the air-filled tube 522, and the heating resistance wire 5242 is fixedly connected to the inside of the heating box 5241.
Referring to fig. 4 and 5, the opening and closing structure 525 includes a connecting rod 5251, a mounting frame 5252, a mounting block 5253, a plug block 5254 and a plurality of pressing rods 5255; mounting block 5253 fixed connection is on the blast pipe 51 inner wall, tapered hole 526 has been seted up to mounting block 5253 up end, chock 5254 slides and connects in tapered hole 526, connecting rod 5251 sets up vertically, connecting rod 5251 lower extreme fixed connection is in chock 5254 up end, mounting frame 5252 fixed connection is in the connecting rod 5251 up end, guipure 112 passes in mounting frame 5252, a plurality of extrusion stem 5255 length direction is parallel with guipure 112 length direction, a plurality of extrusion stem 5255 all fixed connection are in mounting frame 5252 up end.
Referring to fig. 3 and 6, two blocking assemblies 6 for blocking the material passing through holes 33 when the air blowing pipe 51 blows air are arranged in the recycling box 31, the two blocking assemblies 6 correspond to the two material passing through holes 33 one by one, and each blocking assembly 6 comprises a U-shaped frame 61, a blocking door 62 for blocking the material passing through holes 33 and a driving structure 63 for driving the blocking door 62 to move; u type frame 61 fixed connection retrieves on the box 31 inside wall, and U type frame 61 is located the through-material through-hole 33 top, blocks that door 62 vertical sliding connection is between U type frame 61 and the recovery box 31 inner wall.
Referring to fig. 3 and 4, the driving structure 63 includes a reversing gear 631, a fixing rod 632, a driven rack 633, and a driving rack 634; the fixed rod 632 is fixedly connected to the side wall of the connecting rod 5251, the driving rack 634 is vertically arranged, and the driving rack 634 is fixedly connected to one end of the fixed rod 632, which is far away from the connecting rod 5251; the driven rack 633 is vertically arranged, and the upper end face of the driven rack 633 is fixedly connected to the lower end face of the stop gate 62; the reversing gear 631 is rotatably connected to the inner side wall of the recycling bin 31, the reversing gear 631 is located between the driven rack 633 and the driving rack 634, and the reversing gear 631 is engaged with the driven rack 633 and the driving rack 634.
Referring to fig. 3 and 6, a maintaining assembly 7 for maintaining a distance between the blocking door 62 and the frame 1 is disposed between the U-shaped frame 61 and the inner sidewall of the recovery casing 31, and the maintaining assembly 7 includes a maintaining spring 71, a fixing plate 72, a mounting rod 73, and a nut 74; the fixing plate 72 is fixedly connected to the side wall of the stop door 62, the mounting rod 73 is vertically arranged, the lower end of the mounting rod 73 is fixedly connected to the upper end face of the U-shaped frame 61, the upper end face of the mounting rod 73 penetrates through the fixing plate 72, the nut 74 is in threaded connection with the mounting rod 73, the maintaining spring 71 is located between the fixing plate 72 and the nut 74, one end of the maintaining spring 71 is abutted against the nut 74, and the other end of the maintaining spring 71 is abutted against the fixing plate 72.
The implementation principle of the preparation method of the palladium-carbon catalyst for Suzuki coupling reaction in the embodiment of the application is as follows: before use, an operator can adjust the amount of force between the plug 5254 and the tapered bore 526 by turning the nut 74.
During the use, the coconut shell activated carbon enters the hollow ring pipe 22 and the holding pipe 21 under the driving of the mesh belt 112, the second air blower 232 blows the moisture of the coconut shell activated carbon on the mesh belt 112 through the air supply pipe 231 and the air outlet 24, and then the coconut shell activated carbon moves to the recovery box 31 under the driving of the mesh belt 112.
When the coconut shell activated carbon is located in the recycling box body 31, the first air blower 523 continuously blows air to the air bag 521, so that the air pressure in the air bag 521 is increased, when the air pressure in the air bag 521 reaches a certain value, the air bag 521 moves the plunger block 5254 in the vertical upward direction, at the moment, the driving rack 634 also moves along with the plunger block 5254 in the vertical upward direction, the driving rack 634 drives the driven rack 633 to move in the vertical downward direction through the reversing gear 631, so that the blocking door 62 blocks the material passing through hole 33, and the coconut shell activated carbon on the mesh belt 112 is separated to be primarily dispersed; then under the drive of chock 5254, a plurality of squeeze stems 5255 extrude sponge layer 4 for the moisture in sponge layer 4 extrudees to absorbing in the layer, improves the life of sponge layer 4.
When the gas blow pipe 51 is opened, the coconut shell activated carbon on the mesh belt 112 is blown up to the storage hole 42 on the sponge layer 4 by hot gas, so that the drying effect of the sponge layer 4 on the coconut shell activated carbon is better, when part of the coconut shell activated carbon is contradicted with the sponge layer 4, the extrusion rod 5255 extrudes the sponge layer 4 and then recovers, and the water absorption effect of the sponge layer 4 on the coconut shell activated carbon is better.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. A preparation method of a palladium-carbon catalyst for Suzuki coupling reaction is characterized by comprising the following steps:
s1: boiling and activating coconut shell activated carbon by 5-10% dilute nitric acid, washing the activated carbon to be neutral by deionized water, drying and crushing the activated carbon by shaking;
s2: metering the coconut shell activated carbon treated in the step S1, adding the coconut shell activated carbon into an alcohol solution containing a phosphorus ligand for impregnation, wherein the impregnation temperature is controlled to be 50-60 ℃, and then removing the solvent to obtain triphenylphosphine-loaded activated carbon;
s3: pulping the triphenylphosphine-loaded active carbon and tetraammine palladium bicarbonate by using water, ethanol or glycol;
s4: controlling the temperature at 80-100 ℃, and introducing hydrogen to reduce for 3-4h to obtain the palladium-carbon catalyst.
2. A preparation method of a palladium-carbon catalyst for Suzuki coupling reaction is characterized by comprising the following steps: the device for drying and shattering in the S1 comprises a rack (1), wherein a driving assembly (11) for driving a plurality of raw materials to move is arranged on the rack (1), the driving assembly (11) comprises two rotating rollers, a driving motor (111) for driving the rotating rollers to rotate and a mesh belt (112) for blocking the raw materials, the two rotating rollers are rotatably connected to the rack (1), the mesh belt (112) is sleeved on the two rotating rollers, an air blowing assembly (5) for intermittently blowing hot air to the mesh belt (112) is arranged right below the mesh belt (112), and the air blowing assembly (5) comprises an air blowing pipe (51) and an air blowing piece (52) for intermittently blowing air to the air blowing pipe (51); the air blowing pipe (51) and the air blowing piece (52) are arranged on the rack (1).
3. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 2, wherein the palladium-carbon catalyst comprises: the air blowing piece (52) comprises an air bag (521), a first air blower (523) used for continuously inflating the air bag (521), a heating structure (524) used for heating air blown out by the first air blower (523), and an opening and closing structure (525) used for intermittently opening and closing the air bag (521); the air blowing pipe (51) is communicated with the air bag (521), and the opening and closing structure (525) is positioned in the air blowing pipe (51).
4. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 3, wherein the palladium-carbon catalyst comprises: a sponge layer (4) used for storing and absorbing water for the raw materials is arranged on the machine frame (1), the sponge layer (4) is positioned right above the air blowing pipe (51), and a plurality of storage holes (42) used for storing and absorbing water for the raw materials are formed in one end surface, close to the mesh belt (112), of the sponge layer (4); and a water absorption layer is arranged at one end of the sponge layer (4) far away from the mesh belt (112).
5. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 4, wherein the palladium-carbon catalyst comprises: the opening and closing structure (525) comprises a connecting rod (5251), a mounting block (5253), a plug block (5254) and a plurality of extrusion rods (5255); the mounting block (5253) is arranged in the air blowing pipe (51), a tapered hole (526) is formed in one end, far away from the air bag (521), of the mounting block (5253), the plug block (5254) is connected in the tapered hole (526) in a sliding mode and used for blocking the tapered hole (526), one end of the connecting rod (5251) is arranged on the plug block (5254), the extrusion rods (5255) are arranged at one end, far away from the plug block (5254), of the connecting rod (5251), and the extrusion rods (5255) are used for extruding the sponge layer (4).
6. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 5, wherein the palladium-carbon catalyst comprises: the air-drying device is characterized in that an air-drying assembly (2) used for blowing away most of water on a raw material is arranged on the rack (1), the air-drying assembly (2) comprises two holding pipes (21), a hollow ring pipe (22) and an air supply piece (23) used for continuously supplying air to the interior of the hollow ring pipe (22), the hollow ring pipe (22) is located between the two holding pipes (21), the holding pipes (21) are arranged on the hollow ring pipe (22), a plurality of air outlets (24) are formed in the inner wall of the hollow ring pipe (22), and the mesh belt (112) penetrates through the two holding pipes (21) and the interior of the hollow ring pipe (22).
7. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 6, wherein the palladium-carbon catalyst comprises: the frame (1) is provided with a recovery assembly (3) for utilizing redundant hot air discharged by the air bag (521), and the recovery assembly (3) comprises a recovery box body (31) and a recycling pipe (32); the sponge layer (4), the water absorbing layer and the blowing pipe (51) are positioned in the recovery box body (31), and a material through hole (33) for the mesh belt (112) to penetrate through is formed in the recovery box body (31).
8. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 7, wherein the palladium-carbon catalyst comprises: a blocking assembly (6) used for blocking the through-material through hole (33) when the air blowing pipe (51) blows air is arranged in the recovery box body (31), and the blocking assembly (6) comprises a blocking door (62) used for blocking the through-material through hole (33) and a driving structure (63) used for driving the blocking door (62) to move; the stop door (62) is connected to the inner side wall of the recovery box body (31) in a sliding mode.
9. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 8, wherein the palladium-carbon catalyst comprises: block door (62) and slide along connecting rod (5251) glide direction and connect on retrieving box (31) inside wall, drive structure (63) are including reversing gear (631), driven rack (633) and initiative rack (634), driven rack (633) set up block on the door (62), initiative rack (634) sets up on connecting rod (5251), reversing gear (631) are located between driven rack (633) and initiative rack (634), reversing gear (631) rotate connect on retrieving the inside wall of box (31), reversing gear (631) all mesh with driven rack (633) and initiative rack (634).
10. The method for preparing the palladium-carbon catalyst for Suzuki coupling reaction according to claim 9, wherein the palladium-carbon catalyst comprises: a maintaining assembly (7) used for maintaining the distance between the blocking door (62) and the rack (1) is arranged between the blocking door (62) and the rack (1), and the maintaining assembly (7) comprises a maintaining spring (71), an installation rod (73) and a nut (74); the installation pole (73) length direction is parallel with the sliding direction of blocking door (62), it connects in to block door (62) and slide on installation pole (73), nut (74) threaded connection in on installation pole (73), maintain spring (71) cover and locate on installation pole (73), maintain spring (71) and be located nut (74) and block between door (62), it is inconsistent with nut (74) to maintain spring (71) one end, it sets up on blocking door (62) to maintain spring (71) other end.
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