Catalytic method and catalytic equipment for preparing alkanediol

Abstract

The invention discloses a catalysis method and catalysis equipment for preparing alkanediol, and relates to the technical field of catalytic reaction, the catalysis equipment comprises a skid-mounted rack, a main shaft, a plurality of reaction kettles, a plurality of bases, a plurality of middle tanks, a plurality of conical leakage plates and a plurality of annular baffles, the multiple reaction kettles are rotatably connected to the main shaft at equal intervals in the vertical direction, the multiple bases correspond to the reaction kettles and are detachably connected with the reaction kettles, the multiple middle tanks correspond to the reaction kettles and are fixedly connected to the upper sides of the bases, the middle tanks are inserted into the reaction kettles, and heating rods are arranged in the middle tanks. The conical leakage plates are fixedly connected to the outer side of the middle tank in a sleeving mode at equal intervals, the annular baffles correspond to the conical leakage plates, the annular baffles are slidably connected to the outer side of the middle tank in the vertical direction, and the annular baffles are fixedly connected with the conical leakage plates through spring rods. The 1, 2-octane / decanediol is synthesized through catalytic oxidation, the catalyst can be repeatedly used, and the reaction cost is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of catalytic reaction, and particularly relates to a catalytic method for preparing alkylene diol and its catalytic equipment. Background Art

[0002] Alkylene diol is a class of organic compounds containing two hydroxyl (-OH) functional groups, belonging to dihydric alcohols, and is usually connected to the 1st and 2nd carbon atoms of the carbon chain. Such compounds have two hydroxyl groups, which endow them with some unique chemical and physical properties. Alkylene diols have a wide range of applications in multiple fields: Alkylene diols have good hygroscopic and moisturizing properties and are commonly used as humectants and preservatives in cosmetics and have certain antibacterial ability; due to their good solubility and stability, alkylene diols are often used as solvents, and can dissolve some ingredients that are difficult to dissolve in water, such as fragrances and pigments, in the formulation to make the product more uniform and stable; alkylene diols can also be used as antifreeze agents and raw materials for synthesizing polyester fibers. 1,2-Octanediol and 1,2-decanediol are vicinal diols with relatively long carbon chains in alkylene diols, and their synthesis is carried out through catalytic reactions. Usually, a fixed-bed reaction catalytic equipment is selected. A fixed-bed reactor refers to a reactor filled with granular solid catalysts or solid reactants inside to form a stacked bed layer of a certain height. While gas or liquid materials flow through the gaps between the particles and pass through the stationary fixed-bed layer, a heterogeneous reaction process is realized.

[0003] However, for the current fixed-bed reaction catalytic equipment, since the equipment is stationary, when replacing and recovering catalysts for medium and large-scale reaction devices, it is very cumbersome and difficult. It is necessary for workers to enter the reaction kettle to carry out the operations of catalyst replacement and recovery, which not only affects the production and synthesis efficiency, but also has a relatively high labor intensity. Moreover, for medium and large-scale catalytic reaction devices, when heating reactions are carried out, the heating source outside the reaction kettle is far from the central position, resulting in uneven heating. Therefore, a new type of reaction catalytic equipment that is convenient for catalyst replacement is needed to solve the current problems. Summary of the Invention

[0004] In view of the above problems, the present invention provides a catalytic equipment for preparing alkylene diol, including a skid-mounted frame, a main shaft, a plurality of reaction kettles, a plurality of bases, a plurality of intermediate tanks, a plurality of conical leak plates, and a plurality of annular baffles. The main shaft is vertically connected to the skid-mounted frame, and the plurality of reaction kettles are rotatably connected to the main shaft at equal intervals in the vertical direction. The plurality of bases correspond to the reaction kettles, and the bases are detachably connected to the reaction kettles. The plurality of intermediate tanks correspond to the reaction kettles, and the intermediate tanks are fixedly connected to the upper side of the bases. The intermediate tanks are inserted into the interior of the reaction kettles. Heating rods are arranged inside the intermediate tanks. The plurality of conical leak plates are fixedly sleeved on the outer side of the intermediate tanks at equal intervals. The plurality of annular baffles correspond to the conical leak plates, and the annular baffles are slidably connected to the outer side of the intermediate tanks in the vertical direction. The annular baffles are fixedly connected to the conical leak plates through spring rods.

[0005] Furthermore, it also includes multiple heating interlayers and two opposing frames. A heating interlayer is attached to each side of each reactor. The heating interlayer is arc-shaped and connected to an external heater. The two opposing frames are slidably connected to both sides of the skid-mounted frame. Each opposing frame is fixed to an adjacent heating interlayer. The heating interlayer works in conjunction with the heating rod to achieve internal and external heating of the reactor.

[0006] Furthermore, it also includes a driving frame, multiple supporting frames and multiple connecting frames. The driving frame is connected to the main shaft along the axial sliding direction. The multiple supporting frames correspond to the base. The supporting frames are fixedly connected to the base. The supporting frames are rotatably connected to the driving frame. The supporting frames are rotatably connected to the main shaft. After the driving frame moves downward, it drives the base to separate from the reactor. The multiple connecting frames correspond to the reactor. The connecting frames are rotatably connected to the main shaft. The connecting frames are fixedly connected to the outside of the reactor. The connecting frames drive the reactor to rotate, thereby providing space for the separation of the base.

[0007] Furthermore, it also includes a slot, multiple racks, a top rack, a propulsion rack, a first electric cylinder and a second electric cylinder. A slot is opened on the circumferential side of the annular baffle. Multiple racks are respectively located on both sides of the main shaft. The racks correspond to the rotated annular baffle. The racks are inserted into the slots to drive the annular baffle to move up. The annular baffle moves up and separates from the conical leak plate. The top rack connects all the racks. The propulsion rack is slidably connected to the skid-mounted frame. The top rack is slidably connected to the propulsion rack in a vertical direction. The first electric cylinder is connected to the skid-mounted frame. The first electric cylinder pushes the propulsion rack to slide. The second electric cylinder is connected to the propulsion rack. The output shaft of the second electric cylinder is connected to the top rack.

[0008] Furthermore, it also includes multiple first collection tanks and multiple second collection tanks, the multiple first collection tanks correspond one-to-one to the plug-in rack, the first collection tank is connected to the lower side of the plug-in rack, the first collection tank is semicircular, the multiple second collection tanks correspond one-to-one to the first collection tanks, the second collection tanks are detachably connected to the skid-mounted frame, and the first collection tank collects the catalyst after docking with the second collection tank.

[0009] Furthermore, it also includes a first motor and a first screw. The first motor is connected to the skid-mounted frame. The first screw is rotatably connected to the skid-mounted frame. The first screw is a bidirectional screw. Both sides of the first screw pass through the opposing frames respectively. The first screw is threadedly matched with the corresponding opposing frame.

[0010] Furthermore, it also includes a second lead screw, a second motor, multiple rotating cylinders and multiple spur gear groups. The second lead screw is vertically rotatably connected to the skid-mounted frame, the second lead screw penetrates the driving frame, the second lead screw and the driving frame are threadedly matched, the second motor is connected to the skid-mounted frame, the second motor output shaft is fixedly connected to the second lead screw, multiple rotating cylinders correspond to the connecting frame one by one, the rotating cylinders are connected to the skid-mounted frame, multiple spur gear groups correspond to the connecting frame one by one, and the spur gear groups link the corresponding rotating cylinders with the connecting frame.

[0011] Further, it also includes a plurality of quick connectors, a plurality of pipelines, and a plurality of solenoid valves. The plurality of quick connectors are connected to the plurality of pipelines, and adjacent reactors are connected through the quick connectors and pipelines. The pipelines are high-pressure-resistant flexible tubes, and solenoid valves are arranged on the pipelines.

[0012] The present invention also provides a catalytic method for preparing alkanediol, which uses the above catalytic equipment and is characterized by including the following steps: S1. When carrying out the catalytic reaction, a catalyst is filled in the box-shaped structure composed of the annular baffle 8 and the conical leak plate 7. 1-octene / decene and formic acid are introduced into the top inlet of the uppermost reactor 3. The external heater operates, and the heating jacket 10 is heated by steam or heat-conducting oil. The inner heating rod 6 is energized to achieve synchronous and uniform heating inside and outside. It is heated to 60 °C, and hydrogen peroxide is dropped, and the reaction is kept warm for 0.5 h. S2. A 28% sodium hydroxide solution is added to the product of the previous step, stirred at 60 °C for 0.5 h, allowed to stand for stratification, the water layer is removed, the organic layer is washed with water once, the water layer is neutralized with formic acid, and then water is removed through two steps of distillation and centrifugation, and the product sodium formate is obtained after drying. The water layer for washing can be used to prepare the 28% sodium hydroxide solution. S3. Water is obtained by vacuum distillation and is used to prepare the 28% sodium hydroxide solution. The remaining crude product is subjected to vacuum rectification at 134 - 150 °C to obtain 1,2-octene / decene diol.

[0013] The beneficial effects of the present invention are as follows: (1) The present invention can catalytically oxidize and synthesize 1,2-octene / decene diol, and the catalyst can be reused, reducing the reaction cost.

[0014] (2) In the present invention, a box-shaped structure is formed by the conical leak plate and the annular baffle, and the catalyst is filled in this box-shaped structure. When replacing the catalyst, the reactor is rotated along the main axis. When the reactor rotates to the side, the base moves down and separates from the reactor. The central tank, conical leak plate, and annular baffle on the base move down and separate from the reactor, and the box-shaped structure and the catalyst are exposed outside the reactor, facilitating their replacement and recovery; By moving the annular baffle upward to separate it from the conical leak plate, the catalyst quickly slides down on the inclined conical leak plate due to gravity, further realizing the quick replacement and recovery operation of the catalyst and reducing the labor intensity; By arranging the central tank inserted in the middle of the reactor to form a sandwich-like structure with the reactor, and heating rods are arranged in the central tank to achieve synchronous heating inside and outside with the outer heating jacket, the heating is uniform during the reaction process, and thus effectively solves the problems of difficult catalyst recovery and replacement and uneven heating of the reactor in the current reaction catalytic device.

[0015] (3) Drive the propulsion frame forward through the first electric cylinder, so that the insertion frame is inserted into the corresponding card slot. Drive the top frame to move upward through the second electric cylinder, so that the insertion frame moves upward, and then drive all the annular baffles to move upward synchronously, so that the annular baffles are separated from the conical leak plate, and the catalyst automatically slides down quickly. The first collection tank and the second collection tank form a complete collection device, and the catalyst falls into the collection device for collection after sliding down, thereby realizing the automatic catalyst replacement and collection operation. Description of the Drawings

[0016] Figure 1 Schematic diagram of the overall structure of the present invention Figure 1 。

[0017] Figure 2 Schematic diagram of the overall structure of the present invention Figure 2 。

[0018] Figure 3 Schematic diagram of the spindle position of the present invention.

[0019] Figure 4 Schematic diagram of the reaction kettle structure of the present invention.

[0020] Figure 5 Schematic diagram of the structure of the middle tank of the present invention.

[0021] Figure 6 Schematic diagram of the position of the conical leak plate of the present invention.

[0022] Figure 7 Schematic diagram of the structure of the conical leak plate of the present invention.

[0023] Figure 8 Schematic diagram of the position of the heating jacket of the present invention.

[0024] Figure 9 Schematic diagram of the position of the driving frame of the present invention.

[0025] Figure 10 Schematic diagram of the structure of the driving frame of the present invention.

[0026] Figure 11 Schematic diagram of the structure of the insertion frame of the present invention.

[0027] Figure 12 Schematic diagram of the working state of the second collection tank of the present invention.

[0028] Reference numerals: 1, skid-mounted frame; 2, main shaft; 3, reactor; 4, base; 5, intermediate tank; 6, heating rod; 7, conical leak plate; 8, annular baffle; 9, spring rod; 10, heating jacket; 11, opposing frame; 12, driving frame; 13, support frame; 14, connecting frame; 15, card slot; 16, inserting frame; 17, top frame; 18, pushing frame; 19, first electric cylinder; 20, second electric cylinder; 21, first collection tank; 22, second collection tank; 23, first motor; 24, first lead screw; 25, second lead screw; 26, second motor; 27, rotary cylinder; 28, spur gear set; 29, quick connector; 30, pipeline; 31, solenoid valve. Detailed implementation manners

[0029] In order to make the objectives, technical solutions and advantages of the present invention clearer and more understandable, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0030] As Figures 1 - 12 shown, the present invention provides a catalytic device for preparing alkylene glycol, including a skid-mounted frame 1, a main shaft 2, a plurality of reactors 3, a plurality of bases 4, a plurality of intermediate tanks 5, a plurality of conical leak plates 7 and a plurality of annular baffles 8. The main shaft 2 is vertically connected to the skid-mounted frame 1, and the plurality of reactors 3 are rotatably connected to the main shaft 2 at equal intervals in the vertical direction. The plurality of bases 4 correspond to the reactors 3, and the bases 4 are detachably connected to the reactors 3. The plurality of intermediate tanks 5 correspond to the reactors 3, the intermediate tanks 5 are fixedly connected to the upper side of the bases 4, the intermediate tanks 5 are inserted into the reactors 3, heating rods 6 are arranged in the intermediate tanks 5, the plurality of conical leak plates 7 are fixedly sleeved on the outer side of the intermediate tanks 5 at equal intervals, the plurality of annular baffles 8 correspond to the conical leak plates 7, and the annular baffles 8 are slidably connected to the outer side of the intermediate tanks 5 in the vertical direction. The annular baffles 8 are fixedly connected to the conical leak plates 7 through spring rods 9; It further includes a plurality of heating jackets 10 and two opposing frames 11. One heating jacket 10 is attached to each side of each reactor 3. The heating jacket 10 is arc-shaped and is connected to an external heater. The two opposing frames 11 are respectively slidably connected to both sides of the skid-mounted frame 1. Each opposing frame 11 is fixed to the adjacent heating jacket 10. The heating jacket 10 and the heating rod 6 cooperate to work, realizing internal and external heating of the reactor 3.

[0031] In the above embodiments, a box-shaped structure is formed by the conical leak plate 7 and the annular baffle 8, and the catalyst is filled in the box-shaped structure. When replacing the catalyst, the reactor 3 is rotated along the main shaft 2. When the reactor 3 rotates to the side, the base 4 moves down and separates from the reactor 3. The intermediate tank 5, the conical leak plate 7 and the annular baffle 8 on the base 4 move down and separate from the reactor 3, and the box-shaped structure and the catalyst are exposed outside the reactor 3, facilitating their replacement and recovery; The annular baffle 8 is moved upward to separate it from the conical leakage plate 7. The catalyst slides down quickly on the inclined conical leakage plate 7 due to gravity, further realizing the rapid replacement and recovery operation of the catalyst and reducing labor intensity. By arranging a central tank 5 to be inserted in the middle of the reactor 3, a sandwich structure is formed with the reactor 3, and a heating rod 6 is arranged in the central tank 5 to achieve synchronous heating inside and outside with the outer heating interlayer 10, so that the heating is uniform during the reaction process, thereby effectively solving the problem of difficult recovery and replacement of catalysts in the current reaction catalytic device and uneven heating of the reactor 3; The spring rod 9 provides a downward force for the annular baffle 8 so that the annular baffle 8 and the conical drain plate 7 are stably docked.

[0032] The base 4 is sealed when docked with the reactor 3, and adopts the traditional reactor 3 sealing cover connection method, which can be a lever type or a screw type. The heating interlayer 10 is hollow and connected to the external heater through a hose. It is heated by water vapor medium or heat transfer oil medium. The external heater is not described in detail for the sake of clarity of the prior art.

[0033] Specifically, Figure 1 , Figure 9 and Figure 10 As shown, it also includes a driving frame 12, multiple supporting frames 13 and multiple connecting frames 14. The driving frame 12 is axially slidably connected to the main shaft 2. The multiple supporting frames 13 correspond to the base 4. The supporting frames 13 are fixedly connected to the base 4. The supporting frames 13 are rotatably connected to the driving frame 12. The supporting frames 13 are rotatably connected to the main shaft 2. After the driving frame 12 moves downward, it drives the base 4 to separate from the reactor 3. The multiple connecting frames 14 correspond to the reactor 3. The connecting frames 14 are rotatably connected to the main shaft 2. The connecting frames 14 are fixedly connected to the outer side of the reactor 3. The connecting frames 14 drive the reactor 3 to rotate, thereby providing a clearance space for the separation of the base 4.

[0034] In the above embodiment, the up and down movement of the driving frame 12 causes the supporting frame 13 to move up and down, and then drives all the bases 4 to move up and down, thereby realizing the separation operation of the base 4 and the reactor 3. In order to prevent the adjacent reactor 3 from affecting the separation operation of the base 4, a connecting frame 14 is arranged to rotate on the main shaft 2, driving the reactor 3 to rotate on the main shaft 2, so that the adjacent reactors 3 are staggered to both sides to make way for the separation operation of the base 4.

[0035] Specifically, Figure 1 , Figure 2 , Figure 5 , Figure 6 , Figure 11 and Figure 12As shown in the figure, it further includes a card slot 15, a plurality of plug racks 16, a top rack 17, a propulsion rack 18, a first electric cylinder 19 and a second electric cylinder 20. A card slot 15 is provided on the circumferential side of the annular baffle 8. A plurality of plug racks 16 are respectively located on both sides of the main shaft 2. The plug racks 16 correspond to the rotated annular baffle 8. The plug racks 16 are inserted into the card slot 15 to drive the annular baffle 8 to move upward. The annular baffle 8 moves upward to separate from the conical leak plate 7. The top rack 17 connects all the plug racks 16. The propulsion rack 18 is slidably connected to the loader frame 1. The top rack 17 is slidably connected to the propulsion rack 18 in the vertical direction. The first electric cylinder 19 is connected to the loader frame 1. The first electric cylinder 19 pushes the propulsion rack 18 to slide. The second electric cylinder 20 is connected to the propulsion rack 18. The output shaft of the second electric cylinder 20 is connected to the top rack 17; It further includes a plurality of first collection troughs 21 and a plurality of second collection troughs 22. The plurality of first collection troughs 21 correspond to the plug racks 16 one by one. The first collection troughs 21 are connected to the lower sides of the plug racks 16. The first collection troughs 21 are semi-circular. The plurality of second collection troughs 22 correspond to the first collection troughs 21 one by one. The second collection troughs 22 are detachably connected to the loader frame 1. The first collection troughs 21 and the second collection troughs 22 are docked to collect the catalyst.

[0036] In the above embodiments, the first electric cylinder 19 drives the propulsion rack 18 to move forward, so that the plug racks 16 are inserted into the corresponding card slots 15. The second electric cylinder 20 drives the top rack 17 to move upward, so that the plug racks 16 move upward, and then drives all the annular baffles 8 to move upward synchronously, so that the annular baffles 8 are separated from the conical leak plate 7, and the catalyst automatically slides down quickly. The first collection troughs 21 and the second collection troughs 22 form a complete collection device. After the catalyst slides down, it falls into the collection device for collection, thereby realizing the automatic catalyst replacement and collection operation; When the second collection troughs 22 are not in use, they can be detached from the loader frame 1. To improve efficiency, the second collection troughs 22 can be provided with sliding frames and docked with the first collection troughs 21 by manual pushing or electric driving.

[0037] Specifically, as Figure 1 、 Figure 2 and Figure 8 shown, it further includes a first motor 23 and a first lead screw 24. The first motor 23 is connected to the loader frame 1. The first lead screw 24 is rotatably connected to the loader frame 1. The first lead screw 24 is a bidirectional lead screw. Both sides of the first lead screw 24 penetrate through the opposing frames 11 respectively. The first lead screw 24 is in threaded cooperation with the corresponding opposing frames 11.

[0038] In the above embodiments, the first motor 23 drives the first lead screw 24 to rotate, thereby realizing the operation of the two opposing frames 11 approaching or separating from each other, so that the heating interlayers 10 on both sides are attached to or separated from the reaction kettle 3.

[0039] Specifically, as Figure 2 、 Figure 4, Figure 9 and Figure 10 As shown, it further includes a second lead screw 25, a second motor 26, a plurality of rotary cylinders 27 and a plurality of spur gear sets 28. The second lead screw 25 is vertically rotatably connected to the skid loader frame 1. The second lead screw 25 penetrates through the driving frame 12 and is in threaded cooperation with the driving frame 12. The second motor 26 is connected to the skid loader frame 1, and the output shaft of the second motor 26 is fixedly connected to the second lead screw 25. The plurality of rotary cylinders 27 correspond to the connecting frames 14 one by one. The rotary cylinders 27 are connected to the skid loader frame 1. The plurality of spur gear sets 28 correspond to the connecting frames 14 one by one, and the spur gear sets 28 link the corresponding rotary cylinders 27 and the connecting frames 14.

[0040] In the above embodiments, the second motor 26 drives the second lead screw 25 to rotate, thereby realizing the up and down movement operation of the driving frame 12 and the up and down movement operation of all the bases 4. The rotary cylinders 27 drive the corresponding reactors 3 to rotate to the side through the spur gear sets 28 respectively.

[0041] Specifically, as Figure 4 , Figure 5 and Figure 6 shown, it further includes a plurality of quick connectors 29, a plurality of pipelines 30 and a plurality of solenoid valves 31. The plurality of quick connectors 29 and the plurality of pipelines 30. The adjacent reactors 3 are connected through the quick connectors 29 and the pipelines 30. The pipeline 30 is a high-pressure resistant flexible pipe, and a solenoid valve 31 is arranged on the pipeline 30.

[0042] In the above embodiments, the quick connectors 29 are of the high-pressure resistant type, which can achieve quick docking and separation. The pipelines 30 are high-pressure resistant flexible pipes, which are convenient for the rotation and separation operations of each base 4.

[0043] The present invention also provides a catalytic method for preparing alkylene glycol, including the following steps: S1. When carrying out the catalytic reaction, 10 kg of catalyst is filled in the box-shaped structure composed of the annular baffle 8 and the conical leak plate 7. 400 kg of 1-octene / decene and 700 kg of formic acid are introduced into the top inlet of the uppermost reactor 3. The external heater operates, and the heating jacket 10 is heated by steam or heat transfer oil. The inner heating rod 6 is electrified to realize synchronous and uniform heating inside and outside. It is heated to 60 °C, and 243 kg of hydrogen peroxide is dropped, and the reaction is kept warm for 0.5 h; S2. Add 1100 kg of 28% sodium hydroxide solution to the product of the previous step, stir at 60 °C for 0.5 h, stand for stratification, remove the water layer. The organic layer is washed with water once. After the saponified water layer is neutralized with formic acid, water is removed through two steps of distillation and centrifugation, and 450 kg of sodium formate product is obtained after drying. The water layer of the water wash can be used to prepare 28% sodium hydroxide solution; S3. 150 kg of water was obtained by vacuum distillation and used to prepare 28% sodium hydroxide solution. The remaining crude product was subjected to vacuum distillation (134-150 °C) to obtain 380 kg of 1,2-octanediol / decanediol.

[0044] The working principle of the present invention is as follows: when preparing for catalytic reaction, a catalyst is loaded into a box-shaped structure composed of an annular baffle 8 and a conical leak plate 7, a base 4 is docked and sealed with a corresponding reactor 3, so that all reactors 3 are coaxial, adjacent reactors 3 are connected through a quick connector 29 and a pipeline 30, 1-octyl / decene, formic acid, hydrogen peroxide and other reactants are introduced into the top inlet of the uppermost reactor 3 for reaction, and when heating, an external heater is operated to heat the heating interlayer 10 by steam or heat-conducting oil, and an inner heating rod 6 is energized to achieve synchronous and uniform heating inside and outside; After the reaction is completed, the catalyst is recovered or replaced: all electromagnetic valves 31 are closed, all quick connectors 29 are disassembled to separate adjacent reactors 3, the first motor 23 is operated to drive the first screw 24 to rotate, the first screw 24 drives the opposing frames 11 on both sides to move away from each other, and the heating interlayers 10 on both sides of the reactor 3 move away from each other, so that the reactor 3 can be rotated; The rotating cylinder 27 is operated to drive the spur gear set 28, and the spur gear set 28 drives the connecting frame 14, thereby driving the reactor 3, the base 4 and the components on the base 4 to rotate synchronously. At this time, the support frame 13 rotates with the base 4, and the support frame 13 and the driving frame 12 rotate relative to each other. Then, the adjacent reactors 3 are staggered and located on both sides. The sealing component between the base 4 and the reactor 3 is disassembled (the sealing method adopts the existing technology: lever type or screw type), so that the base 4 and the reactor 3 can be separated; Then, the second motor 26 is operated to drive the second lead screw 25 to rotate, and the second lead screw 25 causes the driving frame 12 to move downward, and the driving frame 12, the supporting frame 13, and the base 4 are synchronously moved downward until the base 4 is separated from the reactor 3. At this time, the annular baffle 8, the conical leakage plate 7, the intermediate tank 5, and the catalyst are exposed to the outside, and the first electric cylinder 19 is operated to push the propulsion frame 18 forward, and the propulsion frame 18 moves forward synchronously with the top frame 17 and the plug-in frame 16, and the plug-in frame 16 is inserted into the card slot 15 of the annular baffle 8, and the first collecting tank 21 moves forward synchronously and fits the outside of the intermediate tank 5. , and then connect the second collecting tank 22, the second collecting tank 22 is docked with the first collecting tank 21, and then the second electric cylinder 20 pushes the top frame 17 to move up, the top frame 17 drives the plug-in frame 16 to move up, the plug-in frame 16 drives the annular baffle 8 to move up, the annular baffle 8 is separated from the conical leakage plate 7, and a gap is leaked between the two. Due to the action of gravity, the catalyst slides quickly from the gap, and the sliding catalyst falls into the first collecting tank 21 and the second collecting tank 22. A collection bag is set at the bottom of the second collecting tank 22 or a collection box is assembled, and the catalyst can be collected manually.

[0045] The above are only the preferred embodiments of the present invention, and are not intended to limit the protection scope of the present invention.

Claims

1. A catalytic device for preparing alkylene glycol, comprising a skid-mounted frame (1), characterized in that, It also includes: A main shaft (2), vertically connected to the skid-mounted machine frame (1); A plurality of reaction kettles (3), rotatably connected to the main shaft (2) at equal intervals in the vertical direction; A plurality of bases (4), corresponding to the reaction kettles (3), the bases (4) being detachably connected to the reaction kettles (3); A plurality of intermediate tanks (5), corresponding to the reaction kettles (3), the intermediate tanks (5) being fixedly connected to the upper side of the bases (4), the intermediate tanks (5) being inserted into the interior of the reaction kettles (3), and heating rods (6) being provided inside the intermediate tanks (5); A plurality of conical filter plates (7), fixedly sleeved on the outer side of the intermediate tanks (5) at equal intervals; A plurality of annular baffles (8), corresponding to the conical filter plates (7), the annular baffles (8) being slidably connected to the outer side of the intermediate tanks (5) in the vertical direction, and the annular baffles (8) being fixedly connected to the conical filter plates (7) through spring rods (9).

2. The catalytic device for preparing alkylene glycol according to claim 1, characterized in that, It also includes: A plurality of heating interlayers (10), one heating interlayer (10) being attached to each side of each reaction kettle (3), the heating interlayers (10) being arc-shaped, and the heating interlayers (10) being connected to an external heater; Two opposing frames (11), respectively slidably connected to both sides of the skid-mounted machine frame (1), each opposing frame (11) being fixed to the adjacent heating interlayer (10); The heating interlayers (10) cooperate with the heating rods (6) to heat the reaction kettles (3) both internally and externally.

3. The catalytic device for preparing alkanediol according to claim 1, characterized in that, It also includes: A driving frame (12), axially slidably connected to the main shaft (2); A plurality of support frames (13), corresponding to the bases (4), the support frames (13) being fixedly connected to the bases (4), the support frames (13) being rotatably connected to the driving frame (12), and the support frames (13) being rotatably connected to the main shaft (2); After the driving frame (12) moves downward, it drives the base (4) to separate from the reaction kettle (3); A plurality of connecting frames (14), corresponding to the reaction kettles (3), the connecting frames (14) being rotatably connected to the main shaft (2), and the connecting frames (14) being fixedly connected to the outer side of the reaction kettles (3); The connecting frames (14) drive the reaction kettles (3) to rotate, providing a clearance space for the separation of the bases (4).

4. The catalytic device for preparing alkanediol according to claim 1, characterized in that, It also includes: A card slot (15), the card slot (15) being provided on the circumferential side of the annular baffle (8); A plurality of insertion frames (16), respectively located on both sides of the main shaft (2), the insertion frames (16) corresponding to the rotated annular baffles (8); The insertion frames (16) are inserted into the card slots (15) to drive the annular baffles (8) to move upward, and the annular baffles (8) move upward to separate from the conical filter plates (7); A top frame (17), connecting all the insertion frames (16); A propulsion frame (18), slidably connected to the skid-mounted machine frame (1), and the top frame (17) being slidably connected to the propulsion frame (18) in the vertical direction; A first electric cylinder (19), connected to the skid-mounted machine frame (1), and the first electric cylinder (19) pushing the propulsion frame (18) to slide; The second electric cylinder (20) is connected to the propulsion frame (18), and the output shaft of the second electric cylinder (20) is connected to the top frame (17).

5. The catalytic device for preparing alkylene glycol according to claim 4, characterized in that, It further includes: A plurality of first collection grooves (21), corresponding to the plug-in frames (16) one by one. The first collection grooves (21) are connected to the lower sides of the plug-in frames (16), and the first collection grooves (21) are semi-circular. A plurality of second collection grooves (22), corresponding to the first collection grooves (21) one by one. The second collection grooves (22) are detachably connected to the skid-mounted machine frame (1). After the first collection grooves (21) are docked with the second collection grooves (22), the catalyst is collected.

6. The catalytic device for preparing alkanediol according to claim 2, characterized in that, It further includes: The first motor (23) is connected to the skid-mounted machine frame (1). The first lead screw (24) is rotatably connected to the skid-mounted machine frame (1). The first lead screw (24) is a bidirectional lead screw. Both sides of the first lead screw (24) penetrate the opposing frame (11) respectively, and the first lead screw (24) is in threaded cooperation with the corresponding opposing frame (11).

7. The catalytic device for preparing alkylene glycol according to claim 3, characterized in that, It further includes: The second lead screw (25) is vertically and rotatably connected to the skid-mounted machine frame (1). The second lead screw (25) penetrates the driving frame (12), and the second lead screw (25) is in threaded cooperation with the driving frame (12). The second motor (26) is connected to the skid-mounted machine frame (1), and the output shaft of the second motor (26) is fixedly connected to the second lead screw (25). A plurality of rotary cylinders (27), corresponding to the connecting frames (14) one by one. The rotary cylinders (27) are connected to the skid-mounted machine frame (1). A plurality of spur gear sets (28), corresponding to the connecting frames (14) one by one. The spur gear sets (28) realize the linkage between the corresponding rotary cylinders (27) and the connecting frames (14).

8. A catalytic apparatus for preparing alkylene glycol according to claim 1, characterized in that, It further includes: A plurality of quick connectors (29) and a plurality of pipelines (30). Adjacent reactors (3) are connected through the quick connectors (29) and the pipelines (30). The pipelines (30) are high-pressure-resistant flexible hoses. A plurality of solenoid valves (31) are provided on the pipelines (30).

9. A catalytic method for preparing alkylene glycol, using the catalytic device according to any one of claims 1-8, characterized in that, It includes the following steps: S1. When carrying out the catalytic reaction, the catalyst is filled in the box-shaped structure composed of the annular baffle 8 and the conical leakage plate 7. 1-octene / decene and formic acid are introduced into the top inlet of the uppermost reactor 3. The external heater operates, and the heating jacket 10 is heated by steam or heat transfer oil. The inner heating rod 6 is energized to achieve synchronous and uniform heating inside and outside. It is heated to 60 °C, and hydrogen peroxide is added dropwise, and the reaction is kept warm for 0.5 h. S2. Add 28% sodium hydroxide solution to the product of the previous step, stir at 60 °C for 0.5 h, stand for layering, remove the water layer. The organic layer is washed with water once. After the water layer is neutralized with formic acid, water is removed through two steps of distillation and centrifugation, and the product sodium formate is obtained after drying. The water layer for washing can be used to prepare 28% sodium hydroxide solution. S3. Water is obtained by vacuum distillation and is used to prepare 28% sodium hydroxide solution. The remaining crude product is subjected to vacuum rectification at 134 - 150 °C to obtain 1,2-octene / decene diol.

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